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Proceedings of the Society of Public Analysts and other Analytical Chemists |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 207-207
Preview
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PDF (73KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700207
出版商:RSC
年代:1932
数据来源: RSC
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| 2. |
Anniversary dinner |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 208-209
Preview
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PDF (178KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700208
出版商:RSC
年代:1932
数据来源: RSC
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| 3. |
Annual Report of Council.March, 1932 |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 209-212
Preview
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PDF (335KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity.CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C.of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700209
出版商:RSC
年代:1932
数据来源: RSC
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| 4. |
Annual address of the President |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 213-219
J. T. Dunn,
Preview
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PDF (699KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity.CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C.of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view.Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned.Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium.Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms.of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view.Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium.Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C.of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700213
出版商:RSC
年代:1932
数据来源: RSC
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| 5. |
A micro-method for the determination of uronic anhydride groups in pectic substances |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 220-223
Harold William Buston,
Preview
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PDF (353KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity.CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C.of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700220
出版商:RSC
年代:1932
数据来源: RSC
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| 6. |
Mohler's test for benzoic acid |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 224-232
Edward T. Illing,
Preview
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PDF (781KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity.CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C.of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view.Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned.Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium.Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms.of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view.Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium.Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C.of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms.give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium.Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes.Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium.Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700224
出版商:RSC
年代:1932
数据来源: RSC
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The composition of linseed oil |
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Analyst,
Volume 57,
Issue 673,
1932,
Page 233-244
N. E. Cocchinaras,
Preview
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PDF (914KB)
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity.CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C.of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view.Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned.Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium.Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms.of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view.Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium.Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C.of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms.give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation.Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium.Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm.up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes.Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium.Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline.Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present.Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms.of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C.of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide.A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm.Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C.the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters.It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700233
出版商:RSC
年代:1932
数据来源: RSC
|
| 8. |
Notes |
| |
Analyst,
Volume 57,
Issue 673,
1932,
Page 244-245
Catherine Eleanor Mallen,
Preview
|
PDF (146KB)
|
|
摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700244
出版商:RSC
年代:1932
数据来源: RSC
|
| 9. |
Notes from the Reports of Public Analysts |
| |
Analyst,
Volume 57,
Issue 673,
1932,
Page 245-247
H. H. Bagnall,
Preview
|
PDF (184KB)
|
|
摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700245
出版商:RSC
年代:1932
数据来源: RSC
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Analyst,
Volume 57,
Issue 673,
1932,
Page 247-249
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摘要:
294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected.The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results.The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable.The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm.Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm. of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected.Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased. The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm.in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic.This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.294 EVERS: THE DETECTION OF SMALL QUANTITIES OF CALCIUM Adding 5 mgrms. of calcium. Added salts. Result. No added salt. Immediate pptn. Sodium chloride, 1 grm. Borax, 1 grm. Sodium potassium tartrate, 1 grm. Potassium citrate, 1 grm. Variations in the concentration of the reagents did not appreciably improve matters. It was found that even 0.25 grm.of potassium citrate in 60 C.C. of solution prevented the precipitation of 2 mgrms. of calcium. Further complications would be introduced if magnesium were also present in the salt as an impurity. CALCIUM OLEATE TEsT.-The formation of an opalescence on the addition of sodium oleate solution to a solution is an extremely delicate test for calcium. Under the best conditions 0.01 mgrm. of calcium in 50 C.C. of solution, or 0.00002 per cent., can just be detected. The test is also, of course, a test for magnesium, but is much less sensitive, 0-6 mgrm. in 50 C.C. of solution, or 0-0012 per cent., being the minimum quantity which can be detected. Further, within certain limits of concentration the pre- cipitation of magnesium is entirely suppressed in the presence of potassium citrate, whilst the sensitiveness of the calcium test is actually increased.The best conditions for the detection of calcium were found to be as follows: Take 50 C.C. of the solution containing calcium, which should be neutral or slightly alkaline. Dissolve in it 2 grms. of potassium citrate, and add 0-3 C.C. of a solution prepared by dissolving 10 grms. of oleic acid in 200 C.C. of 1 per cent. sodium hydroxide. A certain excess of alkali is desirable for the best results. The test is only satisfactory between certain limits of calcium concentration. With quantities exceeding 1 mgrm. in 60 C.C. the opalescence is actually reduced. Under the above conditions quantities of mag- nesium up to 15 mgrms. give no opalescence. Summarising the results, the oleate test is excellent for quantities of calcium varying from 0-01 mgrm. up to 1 mgrm. in the absence of more than 10 mgrms. of magnesium, and within these limits in the absence of other salts the opalescence appears proportional to the calcium present. Further experiments showed, however, that, in spite of its delicacy, the oleate test is not suitable for the purpose in view. Possibly, if the test could be carried out, using standards containing the same concentration of the same salt, it would be satisfactory, but this is hardly practicable. The addition of other salts, even in the absence of potassium citrate, caused the results to be erratic. This was partly due to their “salting out ” effect on the soap, which sometimes caused flocculation, but this was not the whole explanation. Almost immediate pptn. Slight ppt. after 30 minutes. Slight ppt. after 30 minutes. No ppt. This line of investigation was therefore abandoned. Mix and allow the mixture to stand. An excess of the reagent gives less opalescence.
ISSN:0003-2654
DOI:10.1039/AN9325700247
出版商:RSC
年代:1932
数据来源: RSC
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