CN104049058B - A kind of eider down oxygen utilization high precision measurement method - Google Patents
A kind of eider down oxygen utilization high precision measurement method Download PDFInfo
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Abstract
The present invention relates to a kind of eider down oxygen utilization high precision measurement method, it is characterized in that: adopt the potassium permanganate standard solution of two kinds of concentration to replace titration, then press formulae discovery eider down oxygen utilization.Adopt the present invention's two kinds of concentration potassium permanganate standard solution to replace titrimetry, eider down sample oxygen utilization can be detected exactly, compared with original method, while taking into account testing efficiency, substantially increase method measuring accuracy.
Description
Technical field
The present invention relates to a kind of eider down oxygen utilization high precision measurement method, belong to fiber product detection technique field.
Background technology
China has become eider down maximum in the world and production of articles state, country of consumption, and be also maximum exported country, export trade amount occupies the share in eider down market, the world 80%, and eider down market, the world has very important status.
Eider down oxygen utilization and microorganism are all crucial test items, and oxygen utilization and microorganism exist certain relation, reflection be that aerobic microorganism is by the amount of breathing consumed oxygen in water.GB/T 14272 and GB/T 17685 all specifies, when eider down oxygen utilization index is more than 10mg/100g, just to carry out microbiological indicator detection.
Eider down oxygen utilization is as the testing advanced index of eider down microorganism, the accuracy of test seems particularly important, and existing eider down oxygen utilization method of testing adopts a kind of potassium permanganate standard solution titration of concentration, there is the problems such as measuring accuracy is low, data fluctuations is large, and eider down sample oxygen utilization numerical value is less, data fluctuations is larger, and when eider down oxygen utilization test data is less than 3mg/100g, data fluctuations amplitude even reaches more than 20%.
Prior art GB/T 14272-2011 appendix C .7 oxygen utilization measures, GB/T 10288-2003 the 6.5th part: oxygen utilization measures, FZ/T 80001-2002 the 9th part: oxygen utilization measures, a kind of concentration 0.02mol/l potassium permanganate is all adopted to carry out titration, there is the problems such as measuring accuracy is low, data fluctuations is large, and eider down sample oxygen utilization numerical value is less, data fluctuations is larger, when eider down oxygen utilization test data is less than 3mg/100g, data fluctuations amplitude even reaches more than 20%.But applicant finds: the potassium permanganate standard solution adopting two kinds of variable concentrations, the titration step specified according to the present invention, test eider down sample oxygen utilization, can take into account testing efficiency and precision two aspect, measuring accuracy controls within 5%.
Adopt the present invention's two kinds of concentration potassium permanganate standard solution to replace titrimetry, eider down sample oxygen utilization can be detected exactly, compared with original method, while taking into account testing efficiency, substantially increase method measuring accuracy.
The present invention is optimized from aspects such as eider down oxygen utilization test oscillation time, shaking bath temperature, liquor potassic permanganate concentration, titration temperatures, adopt the potassium permanganate standard solution of two kinds of variable concentrations, according to the titration step that the present invention specifies, test eider down sample oxygen utilization, testing efficiency and precision two aspect can be taken into account, measuring accuracy improves greatly, can control within 5%.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, provide a kind of eider down oxygen utilization high precision measurement method, the method can take into account testing efficiency and precision two side.
The object of the present invention is achieved like this:
A kind of eider down oxygen utilization high precision measurement method, described method adopts chemical reagent: potassium permanganate standard solution, sulfuric acid; Treatment conditions are: 0.02mol/l potassium permanganate standard solution, 0.002mol/l potassium permanganate standard solution, 3mol/l sulfuric acid, vibration temperature 20-40 DEG C, duration of oscillation 30-60min, oscillation frequency 150 turns/min, titration temperature 20-40 DEG C, bath raio 1:100; Test procedure: take eider down sample lOg on balance, put into the Erlenmeyer flask of 3000mL, add 1O00mL tertiary effluent, bath raio 1:100; After eider down is soaked, horizontal oscillations 30-60min, oscillation frequency 150 turns/min; Enter in large beaker stand-by with standard sieving after vibration, can not squeeze and filter thing when filtration; 1OOmL tertiary effluent and 3mol/l sulfuric acid 2mL is added in Erlenmeyer flask, make it in acid, with minimum division value 0.01ml microburette instillation 0.002mol/l liquor potassic permanganate one, make it pinkiness, this is the blank sample of contrast, record consume the milliliter number V of potassium permanganate
0; With pipette, extract lOOmL filtrate in Erlenmeyer flask, amount to two parts, respectively add 3mol/l sulfuric acid 2mL; To first part of filtrate, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution shaking, until the pink of solution in control sample after 1min, record consume the milliliter number V of liquor potassic permanganate
1; To second part of filtrate, in two steps titration, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution (V
1-0.01) milliliter, then with microburette instillation 0.002mol/L Standard Potassium Permanganate Solution, until the pink of solution in control sample after 1min, record consume the milliliter number V of liquor potassic permanganate
2; Calculate eider down sample oxygen utilization.
Concrete grammar comprises the steps:
(1) .3mol/l sulfuric acid solution preparation: get the 100ml concentrated sulphuric acid (1.84g/ml), add in the water of 500ml, be mixed with 3mol/l sulfuric acid solution;
(2) .0.02mol/l liquor potassic permanganate preparation: take 3.3g potassium permanganate, be dissolved in 1050ml water, boil 20-30min, cool rear sand filters, filtrate is airtight to be stored in brown bottle;
(3) .0.002mol/l liquor potassic permanganate preparation: 0.02mol/l liquor potassic permanganate is diluted 10 times stand-by, now with the current;
(4). sampling: get two parts of 10g ± 0.1g eider down samples;
(5). eider down sample is put into the Erlenmeyer flask of 3000mL, add 1O00mL tertiary effluent, bath raio 1:100;
(6). after eider down sample is soaked, horizontal oscillations 30-60min, oscillation frequency 150 turns/min;
(7). enter in large beaker stand-by with standard sieving, can not squeeze and filter thing when filtering;
(8). in Erlenmeyer flask, add 1OOmL tertiary effluent and 3mol/l sulfuric acid 2mL, make it in acid, with minimum division value 0.01ml microburette instillation 0.002mol/l liquor potassic permanganate one, make it pinkiness, this is the blank sample of contrast, record consume the milliliter number V of potassium permanganate
0;
(9). with pipette, extract lOOmL filtrate in Erlenmeyer flask, amount to two parts, respectively add 3mol/l sulfuric acid 2mL;
(10). to first part of filtrate, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution shaking, until the pink of solution in control sample after 1min, record consume the milliliter number V of 0.02mol/l liquor potassic permanganate
1;
(11). to second part of filtrate, in two steps titration, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution (V
1-0.01) milliliter, then with microburette instillation 0.002mol/L Standard Potassium Permanganate Solution, until the pink of solution in control sample after 1min, record consume the milliliter number V of 0.002mol/l liquor potassic permanganate
2;
(12). repeat step (5)-(11), test second part of eider down sample;
(13). calculate eider down sample oxygen utilization.
Computing formula is as follows:
In formula:
-sample oxygen utilization test result, mg/100ml;
V
0the volume of the 0.002mol/l liquor potassic permanganate that the test of-blank consumes, mL;
V
1the volume of the 0.02mol/l liquor potassic permanganate that-titration 100mL sample liquid consumes, mL;
V
2the volume of the 0.002mol/l liquor potassic permanganate that-titration 100mL sample liquid consumes, mL.
Calculate the average oxygen utilization of two parts of eider down samples.
Compared with prior art, the invention has the beneficial effects as follows:
Embodiment
Below by embodiment, present invention will be further described, but be not limited to lifted embodiment:
Method of testing of the present invention: (the potassium permanganate standard solution of two kinds of variable concentrations replaces titrimetry)
(1) .3mol/l sulfuric acid solution preparation: get the 100ml concentrated sulphuric acid (1.84g/ml), add in the water of 500ml, be mixed with 3mol/l sulfuric acid solution;
(2) .0.02mol/l liquor potassic permanganate preparation: take 3.3g potassium permanganate, be dissolved in 1050ml water, boil 20-30min, cool rear sand filters, filtrate is airtight to be stored in brown bottle;
(3) .0.002mol/l liquor potassic permanganate preparation: 0.02mol/l liquor potassic permanganate is diluted 10 times stand-by, now with the current;
(4). sampling: get two parts of 10g ± 0.1g eider down samples;
(5). eider down sample is put into the Erlenmeyer flask of 3000mL, add 1O00mL tertiary effluent, bath raio 1:100;
(6). after eider down sample is soaked, horizontal oscillations 30-60min, oscillation frequency 150 turns/min;
(7). enter in large beaker stand-by with standard sieving, can not squeeze and filter thing when filtering;
(8). in Erlenmeyer flask, add 1OOmL tertiary effluent and 3mol/l sulfuric acid 2mL, make it in acid, with minimum division value 0.01ml microburette instillation 0.002mol/l liquor potassic permanganate one, make it pinkiness, this is the blank sample of contrast, record consume the milliliter number V of potassium permanganate
0;
(9). with pipette, extract lOOmL filtrate in Erlenmeyer flask, amount to two parts, respectively add 3mol/l sulfuric acid 2mL;
(10). to first part of filtrate, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution shaking, until the pink of solution in control sample after 1min, record consume the milliliter number V of 0.02mol/l liquor potassic permanganate
1;
(11). to second part of filtrate, in two steps titration, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution (V
1-0.01) milliliter, then with microburette instillation 0.002mol/L Standard Potassium Permanganate Solution, until the pink of solution in control sample after 1min, record consume the milliliter number V of 0.002mol/l liquor potassic permanganate
2;
(12). repeat step (5)-(11), test second part of eider down sample;
(13). calculate eider down sample oxygen utilization.
Computing formula is as follows:
In formula:
-sample oxygen utilization test result, mg/100ml;
V
0the volume of the 0.002mol/l liquor potassic permanganate that the test of-blank consumes, mL;
V
1the volume of the 0.02mol/l liquor potassic permanganate that-titration 100mL sample liquid consumes, mL;
V
2the volume of the 0.002mol/l liquor potassic permanganate that-titration 100mL sample liquid consumes, mL.
Battery of tests: the grey duck down of 60%
Embodiment 1:
Adopt the potassium permanganate standard solution of above-mentioned two kinds of variable concentrations to replace the method for testing of titration, get 8 samples and carry out repeated test, test result is in table 1.
Table 1 60% grey duck down repeated measurement data (alternately titrimetry)
| Sequence number | V 1 /mL | V 2 /mL | V 0 /mL | Oxygen utilization/(mg/100g) |
| 1 | 0.08 | 0.05 | 0.01 | 5.92 |
| 2 | 0.08 | 0.04 | 0.02 | 5.76 |
| 3 | 0.08 | 0.03 | 0.01 | 5.76 |
| 4 | 0.08 | 0.06 | 0.01 | 6.00 |
| 5 | 0.08 | 0.04 | 0.02 | 5.76 |
| 6 | 0.08 | 0.05 | 0.01 | 5.92 |
| 7 | 0.08 | 0.05 | 0.02 | 5.84 |
| 8 | 0.08 | 0.04 | 0.01 | 5.84 |
| Mean value | 0.08 | 0.05 | 0.01 | 5.85 |
| Standard deviation | 0.000 | 0.009 | 0.005 | 0.090 |
| CV% | 0.00 | 20.57 | 35.21 | 1.54 |
As shown in Table 1, this sample oxygen utilization mean value is 5.85 mg/100g, and standard deviation is 0.09 mg/100g, CV% value is 1.54%, and data fluctuations is very little.
Comparative example 1--GB/T 14272-2011 appendix C .7 oxygen utilization measures, and adopt a kind of concentration 0.02mol/l potassium permanganate to carry out titration, get 8 samples and carry out repeated test, test result is in table 2.
Table 2 60% grey duck down repeated measurement data (single concentration titration)
| Sequence number | V 1 /mL | V 0 /mL | V 1-V 0 /mL | Oxygen utilization/(mg/100g) |
| 1 | 0.08 | 0.01 | 0.07 | 5.6 |
| 2 | 0.07 | 0.01 | 0.06 | 4.8 |
| 3 | 0.08 | 0.01 | 0.07 | 5.6 |
| 4 | 0.09 | 0.01 | 0.08 | 6.4 |
| 5 | 0.08 | 0.01 | 0.07 | 5.6 |
| 6 | 0.07 | 0.01 | 0.06 | 4.8 |
| 7 | 0.08 | 0.01 | 0.07 | 5.6 |
| 8 | 0.08 | 0.01 | 0.07 | 5.6 |
| Mean value | 0.08 | 0.01 | 0.07 | 5.5 |
| Standard deviation | 0.006 | 0.000 | 0.006 | 0.513 |
| CV% | 8.14 | 0.00 | 9.32 | 9.32 |
As shown in Table 2, this sample oxygen utilization mean value is 5.5 mg/100g, and standard deviation is 0.513 mg/100g, CV% value is 9.32%, and data fluctuations is relatively large.
Second group of test: the white duck down of 80%
Embodiment 2:
Adopt the potassium permanganate standard solution of two kinds of variable concentrations to replace titration, get 8 samples and carry out repeated test, test result is in table 3.
Table 3 80% white duck down repeated measurement data (alternately titrimetry)
| Sequence number | V 1 /mL | V 2 /mL | V 0 /mL | Oxygen utilization/(mg/100g) |
| 1 | 0.05 | 0.05 | 0.01 | 3.52 |
| 2 | 0.05 | 0.04 | 0.02 | 3.36 |
| 3 | 0.05 | 0.03 | 0.01 | 3.36 |
| 4 | 0.05 | 0.06 | 0.01 | 3.60 |
| 5 | 0.05 | 0.04 | 0.02 | 3.36 |
| 6 | 0.05 | 0.05 | 0.01 | 3.52 |
| 7 | 0.05 | 0.05 | 0.02 | 3.44 |
| 8 | 0.05 | 0.04 | 0.01 | 3.44 |
| Mean value | 0.05 | 0.05 | 0.01 | 3.45 |
| Standard deviation | 0.000 | 0.009 | 0.005 | 0.084 |
| CV% | 0.00 | 20.57 | 35.21 | 2.44 |
As shown in Table 3, this sample oxygen utilization mean value is 3.45 mg/100g, and standard deviation is 0.084 mg/100g, CV% value is 2.44%, and data fluctuations is very little.
Comparative example 1--GB/T 14272-2011 appendix C .7 oxygen utilization measures, and adopt a kind of concentration 0.02mol/l potassium permanganate to carry out titration, get 8 samples and carry out repeated test, test result is in table 4.
Table 4 80% white duck down repeated measurement data (single concentration titration)
| Sequence number | V 1 /mL | V 0 /mL | V 1-V 0 /mL | Oxygen utilization/(mg/100g) |
| 1 | 0.05 | 0.01 | 0.04 | 3.2 |
| 2 | 0.04 | 0.01 | 0.03 | 2.4 |
| 3 | 0.04 | 0.01 | 0.03 | 2.4 |
| 4 | 0.06 | 0.01 | 0.05 | 4.0 |
| 5 | 0.04 | 0.01 | 0.03 | 2.4 |
| 6 | 0.05 | 0.01 | 0.04 | 3.2 |
| 7 | 0.06 | 0.01 | 0.05 | 4.0 |
| 8 | 0.04 | 0.01 | 0.03 | 2.4 |
| Mean value | 0.05 | 0.01 | 0.04 | 3.0 |
| Standard deviation | 0.01 | 0.00 | 0.01 | 0.71 |
| CV% | 18.66 | 0.00 | 23.64 | 23.64 |
As shown in Table 4, this sample oxygen utilization mean value is 3.0 mg/100g, and standard deviation is 0.71 mg/100g, CV% value is 23.64%, and data fluctuations is relatively large.
As can be seen from test findings, adopt the present invention's two kinds of concentration potassium permanganate standard solution to replace titrimetry, eider down sample oxygen utilization can be detected exactly, compared with original method, substantially increase method measuring accuracy, measuring accuracy can be controlled within 5%.
Claims (4)
1. an eider down oxygen utilization high precision measurement method, is characterized in that: the potassium permanganate standard solution adopting two kinds of concentration, test eider down sample oxygen utilization; Test procedure comprises:
Add 100mL tertiary effluent and 3mol/l sulfuric acid 2mL in a reservoir, make it in acid, with minimum division value 0.01ml microburette instillation 0.002mol/l liquor potassic permanganate one, make it pinkiness, this is the blank sample of contrast, record consume the milliliter number V of potassium permanganate
0;
Take eider down sample and add tertiary effluent, bath raio 1:100, soak, vibrate, get filtrate; With pipette, extract l00mL filtrate in container, amount to two parts, respectively add 3mol/l sulfuric acid 2mL;
To first part of filtrate, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution shaking, until the pink of solution in control sample after 1min, record consume the milliliter number V of liquor potassic permanganate
1;
To second part of filtrate, in two steps titration, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution (V
1-0.01) milliliter, then with microburette instillation 0.002mol/L Standard Potassium Permanganate Solution, until the pink of solution in control sample after 1min, record consume the milliliter number V of liquor potassic permanganate
2; Calculate eider down sample oxygen utilization;
Computing formula is as follows:
In formula:
-sample oxygen utilization test result, mg/100ml;
V
0the volume of the 0.002mol/l liquor potassic permanganate that the test of-blank consumes, mL;
V
1the volume of the 0.02mol/l liquor potassic permanganate that-titration 100mL sample liquid consumes, mL;
V
2the volume of the 0.002mol/l liquor potassic permanganate that-titration 100mL sample liquid consumes, mL.
2. eider down oxygen utilization high precision measurement method according to claim 1, is characterized in that, the preparation method of described filtrate: take eider down sample, add tertiary effluent by bath raio 1:100; After eider down is soaked, horizontal oscillations 30-60min, oscillation frequency 150 turns/min; Enter in large beaker stand-by with standard sieving after vibration, can not squeeze and filter thing when filtering.
3. eider down oxygen utilization high precision measurement method according to claim 1, is characterized in that, titration temperature 20-40 DEG C.
4. eider down oxygen utilization high precision measurement method according to claim 1, it is characterized in that, described method comprises the steps:
(1) .3mol/l sulfuric acid solution preparation: get the concentrated sulphuric acid that 100ml concentration is 1.84g/ml, add in the water of 500ml, be mixed with 3mol/l sulfuric acid solution;
(2) .0.02mol/l liquor potassic permanganate preparation: take 3.3g potassium permanganate, be dissolved in 1050ml water, boil 20-30min, cool rear sand filters, filtrate is airtight to be stored in brown bottle;
(3) .0.002mol/l liquor potassic permanganate preparation: 0.02mol/l liquor potassic permanganate is diluted 10 times stand-by, now with the current;
(4). sampling: the eider down sample getting two parts of 10g ± 0.1g;
(5). eider down sample is put into the Erlenmeyer flask of 3000mL, add 1O00mL tertiary effluent, bath raio 1:100;
(6). after eider down sample is soaked, horizontal oscillations 30-60min, oscillation frequency 150 turns/min;
(7). enter in large beaker stand-by with standard sieving, can not squeeze and filter thing when filtering;
(8). in Erlenmeyer flask, add 100mL tertiary effluent and 3mol/l sulfuric acid 2mL, make it in acid, with minimum division value 0.01ml microburette instillation 0.002mol/l liquor potassic permanganate one, make it pinkiness, this is the blank sample of contrast, record consume the milliliter number V of potassium permanganate
0;
(9). with pipette, extract 100mL filtrate in Erlenmeyer flask, amount to two parts, respectively add 3mol/l sulfuric acid 2mL;
(10). to first part of filtrate, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution shaking, until the pink of solution in control sample after 1min, record consume the milliliter number V of 0.02mol/l liquor potassic permanganate
1;
(11). to second part of filtrate, in two steps titration, with microburette instillation 0.02mol/L Standard Potassium Permanganate Solution (V
1-0.01) milliliter, then with microburette instillation 0.002mol/L Standard Potassium Permanganate Solution, until the pink of solution in control sample after 1min, record consume the milliliter number V of 0.002mol/l liquor potassic permanganate
2;
(12). repeat step (5)-(11), test second part of eider down sample;
(13). calculate eider down sample oxygen utilization.
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|---|---|---|---|---|
| FI98764B (en) * | 1996-01-24 | 1997-04-30 | Keskuslaboratorio | Method for determining a sample's chemical oxygen consumption |
| CN102323376A (en) * | 2011-08-24 | 2012-01-18 | 厦门隆力德环境技术开发有限公司 | Metering parameter correction method of permanganate index water quality analyzer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI98764B (en) * | 1996-01-24 | 1997-04-30 | Keskuslaboratorio | Method for determining a sample's chemical oxygen consumption |
| CN102323376A (en) * | 2011-08-24 | 2012-01-18 | 厦门隆力德环境技术开发有限公司 | Metering parameter correction method of permanganate index water quality analyzer |
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Effective date of registration: 20210629 Address after: No. 188, East Outer Ring Road, Jiangyin high tech Zone, Wuxi City, Jiangsu Province Patentee after: Jiangsu Chengxin Inspection Certification Co.,Ltd. Address before: No. 188, East Outer Ring Road, Jiangyin City, Wuxi City, Jiangsu Province Patentee before: JIANGSU JIANGYIN FIBRES TESTING INSTITUTE |
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| CP01 | Change in the name or title of a patent holder |
Address after: No. 188, East Outer Ring Road, Jiangyin high tech Zone, Wuxi City, Jiangsu Province Patentee after: Jiangsu Chengxin Inspection, Testing and Certification Co.,Ltd. Address before: No. 188, East Outer Ring Road, Jiangyin high tech Zone, Wuxi City, Jiangsu Province Patentee before: Jiangsu Chengxin Inspection Certification Co.,Ltd. |