CN102721757A - Method for detecting residual quantity of perfluoroalkylation compounds in cosmetics - Google Patents
Method for detecting residual quantity of perfluoroalkylation compounds in cosmetics Download PDFInfo
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- CN102721757A CN102721757A CN2012101938316A CN201210193831A CN102721757A CN 102721757 A CN102721757 A CN 102721757A CN 2012101938316 A CN2012101938316 A CN 2012101938316A CN 201210193831 A CN201210193831 A CN 201210193831A CN 102721757 A CN102721757 A CN 102721757A
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Abstract
The invention discloses a method for detecting the residual quantity of perfluoroalkylation compounds in cosmetics. The method is characterized in that compositions to be detected are separated from large quantities of base materials in a cosmetic sample by extracting and purifying steps, and the compositions to be detected are further separated from other compositions which interfere with measurement, and are purified by means of purification, so that the problem that detection cannot be carried out due to excessive interferences is solved. The method is advanced, is good in precision and repeatability, and can be used for comprehensively detecting the perfluoroalkylation compounds in the cosmetics.
Description
Technical field
The present invention discloses the detection method of all-fluoroalkyl compound residual quantity in a kind of cosmetics, belongs to the method for determining chemical technical field.
Background technology
The kind of all-fluoroalkyl compound comprises perfluor caproic acid, perfluoro caprylic acid, perfluoro-pelargonic acid, perfluoro decanoate, perfluor undecanoic acid, perfluor dodecoic acid, perfluorinated butane sulfonic acid, perflexane sulfonic acid, PFOS, perfluoro decane sulfonic acid in the cosmetics that the present invention relates to; Above-mentioned substance in use; Human body is existed harm, prove through present toxicological test, the toxicity of all-fluoroalkyl compound still is very important; If the mankind are exposed in the fluorocarbon surfactant for a long time; Have acute or chronic toxicity, can cause systemic effect because oral, suction or skin infiltrate, the part contact can cause local effect.Particularly the toxicity of this type of material has fatal characteristics; Be nontoxic or compound that toxicity is little does not have very big difference with strong toxic chemical on chemical constitution; That is to say their the also rule of non-structure-toxicity; The toxicity of all compounds all needs could confirm through toxicological test, has increased difficulty for the judgement of this type material toxicity thus.At present can detected PFACs in the environment have multiple, like PFOS (PFOS), perfluoro caprylic acid (PFOA), perflexane sulfonic acid (PFHxS), perfluoro-pelargonic acid (PFNA), perfluoro-heptanoic acid (PFHpA) etc.
Some developed countries have begun to pay attention to the influence of all-fluoroalkyl compound compounds to environment and human health, and have begun to start some related measures and limit its use with relevant laws and regulations, and the situation of limiting the quantity of is seen table 1.According to the Generally Recognized as safe standard under the 2004/1935/EC of the European Union instruction (with the resolution of the material and the material of Food Contact), the PFOA use that is under an embargo.In August, 2005; World Trade Organization (WTO) issue international trade technology barriers circular: the Swedish government (circular number: G/TBT/N/SWE/51) that on July 6th, 2005 notified; Regulation PFOS forbids throwing in Sweden market or supplies specialty to use with the material that can be degraded to PFOS; This motion came into force according to different compound situation between January 1 to 1 day January in 2010 in 2007.On Dec 27th, 2006; European Parliament and council of ministers unite issue " about the instruction of sale of restriction PFOS and use " (2006/122/EC), stipulate that the PFOS content in the all-fluoroalkyl compound must not be above 0.005% in the manufactured goods on the European Union market; Must not surpass 0.1% in the semi-manufacture; Must not surpass 1 μ g/m in textile or the coating
2Norway pollution control management office has issued the ban PoHS instruction of forbidding in consumer products, using some objectionable impurities in the recent period, and this instructs and comes into force on January 1st, 2008, and limiting the quantity of of PFOA of suggestion is 0.005 %, textile or other coating material 1 μ g/m
2" Convention of Stockholm " formally listed PFOS in the persistence organic pollutant list in 2009.
Do not see at present the report of coherent detection all-fluoroalkyl compound method.
Because the variety classes cosmetics in manufacturing process, have added heterogeneity and a large amount of auxiliary materials, wherein with organic principle in the highest flight; Cause the cosmetic base more complicated,, just must test substance be separated from matrix if will satisfy the specificity of assay method and the requirement of sensitivity; And reach certain purity and concentration, promptly require and instrument is played a protective role through extracting and purify two parts pre-treatment step, reach to detect; Otherwise, can't detect owing to disturb too much.
Summary of the invention
The present invention provides the detection method of all-fluoroalkyl compound residual quantity in a kind of cosmetics, is used for the quality control of cosmetics all-fluoroalkyl compound, is used for the total quality control to cosmetics.
The present invention discloses a kind of detection method of measuring all-fluoroalkyl compound residual quantity in the cosmetics, may further comprise the steps:
1) sample pre-treatments
Powdery, the emulsus sample extraction
Take by weighing 1 g sample, add about 5 g zeyssatite, be mixed; Put into abstraction pool and extract, fast solvent extraction appearance extraction conditions: sample cell temperature: 80 ℃; Pressure: 1500 psi; Heat time heating time: 5 min; The static extracting time: 5 min; Solvent: methyl alcohol; Flush volume: methyl alcohol (60% sample cell volume); Nitrogen purging: 60 s; Cycle index: 1 time;
After extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5;
The liquid state sample extraction
Take by weighing 1 g sample in 50 mL centrifuge tubes, add 20 mL methyl alcohol, extract 30 min, ultrasonic Extraction 20 min again with the oscillator vibration; Put in the hydro-extractor, with centrifugal 10 min of 10000 r/min; Drawing supernatant concentrates in the bottle in 250 mL; Repeat the said extracted step, merge extract, rotary evaporation in 40 ℃ of water-baths concentrates; With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2% first acid for adjusting pH value to 4-5;
2) purify
The sample liquid that step 1) is handled is transferred in the mixed type weak anionic exchange solid-phase extraction column, uses 25 mmol/L SASs and the 5 mL methyl alcohol drip washing of 5 mL successively, discards leacheate; Use the 0.1 % ammoniacal liquor methanol solution wash-out of 3 mL again, collect eluent; Eluent blows near doing through nitrogen, is settled to 1 mL with methyl alcohol-0.1 % formic acid solution, crosses 0.22 μ m filter membrane, and filtrating feed flow phase chromatogram tandem mass spectrometer carries out qualitative, quantitative and measures;
3) measure
Liquid phase chromatogram condition:
Chromatographic column: Waters C
18, 2.1 * 150 mm; 3.5 μ m, column temperature: 20 ~ 25 ℃; Flow velocity: 0.20 mL/min; Sample size: 10 μ L; Gradient elution;
The mass spectrum condition:
Ionization mode: electron spray ionisation; Negative ion scanning; Multiple-reaction monitoring; Electron spray voltage :-4500 V;
Gas curtain gas: 45 Psi; Atomization gas: 35 Psi; Auxiliary gas: 40 Psi; Collision gas: 6.0 Psi; Ion source temperature: 550.0 ℃; 4) liquid chromatography-tandem mass spectrometry detects and conclusive evidence:
According to the test condition of step 3) to step 2) appearance liquid measure.
Qualitative determination:
Standard solution and appearance liquid are all measured by the condition of afore mentioned rules, if the retention time identical with standard solution has the peak to occur in the appearance liquid, then it are proved conclusively.As consistent through confirmatory analysis tested constituent mass chromatographic peak retention time and standard substance, selected ion all occurs; Simultaneously the abundance ratio of selected ion is consistent with the relative abundance of standard sample material relevant ions, and similarity (is seen table 3) within permissible variation, and then decidable is positive detects for the sample that quilt is proved conclusively.
The maximum allowable offset of table 3 relative abundance of ions of qualitative when conclusive evidence
| Relative abundance of ions | ＞50％ | ＞20% to 50% | ＞10% to 20% | ≤10％ |
| The relative deviation that allows | ±20％ | ±25％ | ±30％ | ±50％ |
2, quantitative measurement
According to tested components contents situation in the detected sample liquid in the sample, choose the close standard operation liquid of response and analyze, must suitably carry out serial dilution for enriched sample.The response of tested component all should be in the instrument linear response range in standard operation liquid and the appearance liquid.Under above-mentioned chromatographic condition, be 2.90 min ~ 18.70 min with reference to retention time, external standard method is quantitative.The multiple-reaction monitoring chromatogram of standard solution is referring to appendix B.
Six, the result calculates and statement
Calculate every kind of all-fluoroalkyl compound content in the sample with the chromatographic data process software or by (1) formula:
In the formula:
X i ---all-fluoroalkyl compound in the sample
iContent, unit are every kilogram (mg/kg) of milligram;
A i ---the peak area of all-fluoroalkyl compound in the appearance liquid;
c i ---all-fluoroalkyl compound in the standard operation liquid
iConcentration, unit is every milliliter of microgram (mg/mL);
V---the final constant volume of appearance liquid, unit are milliliter (mL);
A Is ---all-fluoroalkyl compound in the standard operation liquid
iPeak area;
m---sample weighting amount, unit is gram (g);
f---dilution gfactor.
Result of calculation should be deducted blank value, and all-fluoroalkyl compound content is in acid group, and the result keeps three position effective digitals.
The kind of the all-fluoroalkyl compound that the present invention relates to comprises: perfluor caproic acid, perfluoro caprylic acid, perfluoro-pelargonic acid, perfluoro decanoate, perfluor undecanoic acid, perfluor dodecoic acid, perfluorinated butane sulfonic acid, perflexane sulfonic acid, PFOS, perfluoro decane sulfonic acid.
Good effect of the present invention is:In cosmetics all-fluoroalkyl compound residual quantity was detected; Through extracting and purifying step; Composition to be measured is separated with a large amount of matrix in the cosmetic sample; And composition to be measured is further separated and purifying with the composition of other interference measurements, otherwise, can't detect owing to disturb too much through purifying.Detection method is advanced, and precision and favorable reproducibility can detect the all-fluoroalkyl compound in the cosmetics comprehensively.
Description of drawings:
Fig. 1 is standard solution multiple-reaction monitoring (MRM) chromatogram:
Fig. 2 is perfluor caproic acid among the embodiment 1, PFOS, perfluoro caprylic acid, perfluor undecanoic acid selection chromatography of ions figure;
Perfluorinated butane sulfonic acid, perfluor caproic acid, perflexane sulfonic acid, perfluoro caprylic acid are selected chromatography of ions figure among Fig. 3 embodiment 2;
Perfluoro-pelargonic acid, perfluor undecanoic acid, PFOS, perfluoro decanoate are selected chromatography of ions figure among Fig. 4 embodiment 3;
Perfluorinated butane sulfonic acid, perfluoro-pelargonic acid, perfluoro decane sulfonic acid, perfluor dodecoic acid are selected chromatography of ions figure among Fig. 5 embodiment 4.
Embodiment
For the ease of understanding the present invention, special case is lifted following instance.Its effect is understood that it is to explaination of the present invention but not to the bright any type of restriction of we.
The liquid state sample
1, takes by weighing 1g sample (No. 1, the toner that Liaoning Entry-Exit Inspection and Quarantine Bureau provides) in 50 mL centrifuge tubes, add 20 mL methyl alcohol, extract 30 min, ultrasonic Extraction 20 min again with the oscillator vibration; Put in the hydro-extractor, with centrifugal 10 min of 10000 r/min.Draw supernatant and concentrate repetition said extracted step in the bottle in 250 mL, merge extract, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2% first acid for adjusting pH value to 4-5.
2, after extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5.
Powdery, emulsus sample
Take by weighing 1 g sample (No. 2, the lipstick that Liaoning Entry-Exit Inspection and Quarantine Bureau provides), add about 5 g zeyssatite, be mixed; Put into abstraction pool and extract, fast solvent extraction appearance extraction conditions: sample cell temperature: 80 ℃; Pressure: 1500 psi; Heat time heating time: 5 min; The static extracting time: 5 min; Solvent: methyl alcohol; Flush volume: methyl alcohol (60% sample cell volume); Nitrogen purging: 60 s; Cycle index: 1 time; After extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5;
Embodiment 3
Powdery, emulsus sample
Take by weighing 1 g sample (No. 3, the emulsion that Liaoning Entry-Exit Inspection and Quarantine Bureau provides), add about 5 g zeyssatite, be mixed; Put into abstraction pool and extract, fast solvent extraction appearance extraction conditions: sample cell temperature: 80 ℃; Pressure: 1500 psi; Heat time heating time: 5 min; The static extracting time: 5 min; Solvent: methyl alcohol; Flush volume: methyl alcohol (60% sample cell volume); Nitrogen purging: 60 s; Cycle index: 1 time; After extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5;
Powdery, emulsus sample
Take by weighing 1 g sample (No. 4, the rouge that Liaoning Entry-Exit Inspection and Quarantine Bureau provides), add about 5 g zeyssatite, be mixed; Put into abstraction pool and extract, fast solvent extraction appearance extraction conditions: sample cell temperature: 80 ℃; Pressure: 1500 psi; Heat time heating time: 5 min; The static extracting time: 5 min; Solvent: methyl alcohol; Flush volume: methyl alcohol (60% sample cell volume); Nitrogen purging: 60 s; Cycle index: 1 time; After extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5;
The appearance liquid of embodiment 1 to embodiment 4 is transferred in the mixed type weak anionic exchange solid-phase extraction column, uses 25 mmol/L SASs and the 5 mL methyl alcohol drip washing of 5 mL successively, discard leacheate.Use the 0.1 % ammoniacal liquor methanol solution wash-out of 3 mL again, collect eluent.Eluent blows near doing through nitrogen, is settled to 1 mL with methyl alcohol-0.1 % formic acid solution, crosses 0.22 μ m filter membrane, and filtrating supplies LC-MS/MS to measure.
Measure:
1) liquid phase chromatogram condition
A chromatographic column: Waters C
18, 2.1 * 150 mm; 3.5 μ m, or suitable person;
B column temperature: room temperature;
C flow velocity: 0.20 mL/min;
D sample size: 10 μ L;
E moving phase and condition of gradient elution are seen table 1.
Table 1 moving phase and condition of gradient elution
2) mass spectrum condition
A ionization mode: electron spray ionisation (ESI);
B scan mode: negative ion scanning;
C detection mode: multiple-reaction monitoring (MRM);
D electron spray voltage :-4500 V;
E gas curtain gas (CUR): 45 Psi (0.31 MPa);
F atomization gas (GS1): 35 Psi (0.24 MPa);
G assists gas (GS2): 40 Psi (0.28 MPa);
H collides gas (CAD): 6.0 Psi (0.15 MPa);
I ion source temperature (TEM): 550.0 ℃;
The qualitative ion pair of j, quota ion to, go a bunch voltage, collision energy to see table 2.
The monitoring ion pair of table 2 target compound, remove bunch voltage and collision energy
Liquid chromatography-tandem mass spectrometry detects and conclusive evidence
According to tested component concentration situation in the appearance liquid, the selected close standard operation solution of concentration, standard operation solution with treat that the response of 10 kinds of all-fluoroalkyl compounds in the sample measuring liquid all should be in the range of linearity of instrument detecting.Standard operation solution injects appearance with appearance liquid equal-volume ginseng and measures.Must suitably carry out serial dilution for enriched sample.
1) qualitative determination
Standard solution and appearance liquid are all measured by the condition of afore mentioned rules, if the retention time identical with standard solution has the peak to occur in the appearance liquid, then it are proved conclusively.As consistent through confirmatory analysis tested constituent mass chromatographic peak retention time and standard substance, selected ion all occurs; Simultaneously the abundance ratio of selected ion is consistent with the relative abundance of standard sample material relevant ions, and similarity (is seen table 3) within permissible variation, and then decidable is positive detects for the sample that quilt is proved conclusively.
The maximum allowable offset of table 3 relative abundance of ions of qualitative when conclusive evidence
| Relative abundance of ions | ＞50％ | ＞20% to 50% | ＞10% to 20% | ≤10％ |
| The relative deviation that allows | ±20％ | ±25％ | ±30％ | ±50％ |
2) quantitative measurement
According to tested components contents situation in the detected sample liquid in the sample, choose the close standard operation liquid of response and analyze, must suitably carry out serial dilution for enriched sample.The response of tested component all should be in the instrument linear response range in standard operation liquid and the appearance liquid.Under above-mentioned chromatographic condition, be 2.90 min ~ 18.70 min with reference to retention time, external standard method is quantitative.The multiple-reaction monitoring chromatogram of standard solution is referring to appendix B.
6, the result calculates and statement
Calculate every kind of all-fluoroalkyl compound content in the sample with the chromatographic data process software or by (1) formula:
In the formula:
X i ---all-fluoroalkyl compound in the sample
iContent, unit are every kilogram (mg/kg) of milligram;
A i ---the peak area of all-fluoroalkyl compound in the appearance liquid;
c i ---all-fluoroalkyl compound in the standard operation liquid
iConcentration, unit is every milliliter of microgram (mg/mL);
V---the final constant volume of appearance liquid, unit are milliliter (mL);
A Is ---all-fluoroalkyl compound in the standard operation liquid
iPeak area;
m---sample weighting amount, unit is gram (g);
f---dilution gfactor.
Result of calculation should be deducted blank value, and all-fluoroalkyl compound content is in acid group, and the result keeps three position effective digitals.
The residual value of table 4 embodiment sample
| | Embodiment | 1 detected level (mg/kg) | |
Embodiment 3 detected levels (mg/kg) | |
| Perfluorinated butane sulfonic acid | / | 0.410 | / | 0.106 | |
| Perflexane sulfonic acid | / | 0.255 | / | / | |
| PFOS | 0.329 | / | 0.338 | / | |
| Perfluoro decane sulfonic acid | / | / | / | 0.128 | |
| The perfluor caproic acid | 0.237 | 0.218 | / | / | |
| Perfluoro decanoate | / | / | 0.284 | / | |
| Perfluoro caprylic acid | 0.298 | 0.306 | / | / | |
| Perfluoro-pelargonic acid | / | / | 0.237 | 0.242 | |
| The perfluor undecanoic acid | 0.386 | / | 0.365 | / | |
| The perfluor dodecoic acid | / | / | / | 0.368 |
The accuracy that shows detection method of the present invention through following test:
Test Example 1
Test specimen: No. 1, the standard model that Liaoning Entry-Exit Inspection and Quarantine Bureau provides---toner
Process of the test:
1, takes by weighing 1g sample (No. 1, the toner that Liaoning Entry-Exit Inspection and Quarantine Bureau provides) in 50 mL centrifuge tubes, add 20 mL methyl alcohol, extract 30 min, ultrasonic Extraction 20 min again with the oscillator vibration; Put in the hydro-extractor, with centrifugal 10 min of 10000 r/min.Draw supernatant and concentrate repetition said extracted step in the bottle in 250 mL, merge extract, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2% first acid for adjusting pH value to 4-5.
2, after extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates.With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5.
3, appearance liquid is transferred in the mixed type weak anionic exchange solid-phase extraction column, uses 25 mmol/L SASs and the 5 mL methyl alcohol drip washing of 5 mL successively, discard leacheate.Use the 0.1 % ammoniacal liquor methanol solution wash-out of 3 mL again, collect eluent.Eluent blows near doing through nitrogen, is settled to 1 mL with methyl alcohol-0.1 % formic acid solution, crosses 0.22 μ m filter membrane, and filtrating supplies LC-MS/MS to measure.
Conclusion (of pressure testing):
Adopt this patent method to carry out check and analysis to the all-fluoroalkyl compound in the positive, testing result shows, this method accurately qualitative and quantitative measurement goes out the content of all-fluoroalkyl compound in the sample.
Claims (1)
1. the detection method of all-fluoroalkyl compound residual quantity in the cosmetics may further comprise the steps:
1) sample pre-treatments
Powdery, the emulsus sample extraction
Take by weighing 1 g sample, add about 5 g zeyssatite, be mixed; Put into abstraction pool and extract, fast solvent extraction appearance extraction conditions: sample cell temperature: 80 ℃; Pressure: 1500 psi; Heat time heating time: 5 min; The static extracting time: 5 min; Solvent: methyl alcohol; Flush volume: methyl alcohol (60% sample cell volume); Nitrogen purging: 60 s; Cycle index: 1 time;
After extraction finishes, extract is transferred to 250 mL concentrates in the bottle, rotary evaporation in 40 ℃ of water-baths concentrates;
With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2 % first acid for adjusting pH value to 4-5;
The liquid state sample extraction
Take by weighing 1 g sample in 50 mL centrifuge tubes, add 20 mL methyl alcohol, extract 30 min, ultrasonic Extraction 20 min again with the oscillator vibration; Put in the hydro-extractor, with centrifugal 10 min of 10000 r/min; Drawing supernatant concentrates in the bottle in 250 mL; Repeat the said extracted step, merge extract, rotary evaporation in 40 ℃ of water-baths concentrates; With methanol constant volume to 10 mL, get 1 mL solution in polypropylene centrifuge tube, be diluted with water to 20 mL,, to be clean with 2% first acid for adjusting pH value to 4-5;
2) purify
The sample liquid that step 1) is handled is transferred in the mixed type weak anionic exchange solid-phase extraction column, uses 25 mmol/L SASs and the 5 mL methyl alcohol drip washing of 5 mL successively, discards leacheate; Use the 0.1 % ammoniacal liquor methanol solution wash-out of 3 mL again, collect eluent; Eluent blows near doing through nitrogen, is settled to 1 mL with methyl alcohol-0.1 % formic acid solution, crosses 0.22 μ m filter membrane, and filtrating feed flow phase chromatogram tandem mass spectrometer carries out qualitative, quantitative and measures;
3) measure
Liquid phase chromatogram condition:
Chromatographic column: Waters C
18, 2.1 * 150 mm; 3.5 μ m, column temperature: 20 ~ 25 ℃; Flow velocity: 0.20 mL/min; Sample size: 10 μ L; Gradient elution;
The mass spectrum condition:
Ionization mode: electron spray ionisation; Negative ion scanning; Multiple-reaction monitoring; Electron spray voltage :-4500 V;
Gas curtain gas: 45 Psi; Atomization gas: 35 Psi; Auxiliary gas: 40 Psi; Collision gas: 6.0 Psi; Ion source temperature: 550.0 ℃; 4) liquid chromatography-tandem mass spectrometry detects and conclusive evidence:
According to the test condition of step 3) to step 2) appearance liquid measure.
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