Polymer total dissolved solids vessel

Abstract

A thin film vessel useable in gravimetric methods for measuring the total dissolved solids or total solids in a liquid sample, or the moisture content of a solid sample. The vessel includes a main body formed of a thin walled polymeric material having a melting temperature greater than 180 C. The main body comprises an open top edge and a sealed bottom edge which define an inner cavity configured to hold a volume of liquid, and indicia applied to a portion of the main body, wherein the indicia include a tare weight of the vessel.

Claims

1. A method for testing total dissolved solids in a liquid sample, the method comprising: placing a volume of liquid into a testing vessel, wherein the testing vessel comprises: a main body comprising an open top end and a sealed bottom end to define an inner cavity configured to hold a volume of liquid, wherein the main body comprises a thin walled polymeric material having a melting temperature greater than 180 C.; and an indicia applied to a portion of the main body indicating a tare weight of the testing vessel, wherein the tare weight of the testing vessel comprises a weight of the testing vessel measured after at least one preconditioning step, wherein the at least one preconditioning step comprises heating the testing vessel to at least 180 C. for a first length of time, heating the testing vessel containing the liquid sample for a time sufficient to evaporate the volume of liquid; heating the testing vessel at 180 C. for a second length of time and weighing the testing vessel; and repeating the step of heating the testing vessel at 180 C. for the second length of time and weighing the testing vessel until a subsequently recorded weight of the testing vessel varies by less than 0.5 mg from a previously recorded weight.

2. The method of claim 1, wherein the second length of time comprise a time of one hour.

3. The method of claim 1, wherein the first length of time comprises a time of at least one hour.

4. The method of claim 1, wherein the volume of liquid comprises a volume of less than 150 ml.

5. The method of claim 1, wherein the weight of the testing vessel comprises a weight of between 0.5 grams and 5.0 grams.

6. The method of claim 1, wherein the polymeric material comprises nylon, polyethylene terephthalate, polyethylene, polypropylene, or a combination thereof.

7. The method of claim 1, wherein the wall thickness of the thin walled polymeric material is less than 0.008 inches.

8. A method of producing a vessel useful for gravimetric testing, the method comprising: performing at least one preconditioning step on the vessel, wherein the at least one preconditioning step comprises heating the vessel to at least 180 C. for a specified time and weighing the vessel to obtain a tare weight of the vessel, wherein the vessel comprises: a main body having an open top end and a sealed bottom end to define an inner cavity configured to hold a volume of liquid, wherein the main body comprises a thin walled polymeric material having a melting temperature greater than 180 C.; and applying an indicia to a portion of the main body of the vessel, wherein the indicia include the tare weight of the vessel.

9. The method of claim 8, further comprising: repeating the preconditioning step until subsequent recorded weights of the vessel vary by less than 0.5 mg.

10. The method of claim 8, wherein the tare weight of the vessel comprises a weight of between 0.5 grams and 5.0 grams.

11. The method of claim 8, wherein the vessel has a wall thickness of less than 0.008 inches.

12. The method of claim 1, wherein a value of the tare weight may be subtracted from a value of the subsequently recorded weight to determine a weight of the total dissolved solids in the volume of liquid.

13. A method of producing a vessel useful for gravimetric testing, the method comprising: performing a preconditioning step on the vessel, wherein the preconditioning step comprises heating the vessel to at least 180 C. for a specified time and weighing the vessel, wherein the vessel comprises: a main body having an open top end and a sealed bottom end to define an inner cavity configured to hold a volume of liquid, wherein the main body comprises a thin walled polymeric material having a melting temperature greater than 180 C.; repeating the preconditioning step until a subsequently recorded weight of the vessel varies by less than 0.5 mg from a previously recorded weight, wherein the subsequently recorded weight of the vessel is a tare weight of the vessel; and applying an indicia to a portion of the main body of the vessel, wherein the indicia include the tare weight of the vessel.

14. The method of claim 13, wherein the tare weight of the vessel is a weight of 0.5 grams to 5.0 grams.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) Aspects, features, benefits and advantages of the embodiments herein will be apparent with regard to the following description, appended claims, and accompanying drawings. In the following figures, like numerals represent like features in the various views. It is to be noted that features and components in these drawings, illustrating the views of embodiments of the presently disclosed invention, unless stated to be otherwise, are not necessarily drawn to scale.

(2) FIG. 1 illustrates a thin film high temperature polymeric flat bottom vessel containing water in accordance with certain aspects of the presently disclosed invention;

(3) FIG. 2 illustrates a thin film high temperature polymeric gusseted standup vessel containing water in accordance with certain aspects of the presently disclosed invention; and

(4) FIG. 3 illustrates a thin film high temperature polymeric pillow style three sided vessel containing water in accordance with certain aspects of the presently disclosed invention.

DETAILED DESCRIPTION

(5) In the following description, the present invention is set forth in the context of various alternative embodiments and implementations involving a thin film high temperature polymeric vessel which may be used in gravimetric methods for measuring the total dissolved solids (TDS) or total solids (TS) in a liquid sample, or the moisture content in a solid sample. While the following description discloses numerous exemplary embodiments, the scope of the present patent application is not limited to the disclosed embodiments, but also encompasses combinations of the disclosed embodiments, as well as modifications to the disclosed embodiments.

(6) Various aspects of the thin film high temperature polymeric vessel may be illustrated by describing components that are coupled, attached, and/or joined together. As used herein, the terms coupled, attached, and/or joined are interchangeably used to indicate either a direct connection between two components or, where appropriate, an indirect connection to one another through intervening or intermediate components. In contrast, when a component is referred to as being directly coupled, directly attached, and/or directly joined to another component, there are no intervening elements shown in said examples.

(7) Various aspects of the thin film high temperature polymeric vessel may be illustrated with reference to one or more exemplary implementations. As used herein, the term exemplary means serving as an example, instance, or illustration, and should not necessarily be construed as preferred or advantageous over other variations of the devices, systems, or methods disclosed herein. Optional or optionally means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event occurs and instances where it does not. In addition, the word comprising as used herein means including, but not limited to.

(8) Relative terms such as lower or bottom and upper or top may be used herein to describe one element's relationship to another element illustrated in the drawings. It will be understood that relative terms are intended to encompass different orientations of aspects of the thin wall high temperature polymeric vessel in addition to the orientation depicted in the drawings. By way of example, if aspects of the thin film high temperature polymeric vessel in the drawings are turned over, elements described as being on the bottom side of the other elements would then be oriented on the top side of the other elements as shown in the relevant drawing. The term bottom can therefore encompass both an orientation of bottom and top depending on the particular orientation of the drawing.

(9) It must also be noted that as used herein and in the appended claims, the singular forms a, an, and the include the plural reference unless the context clearly dictates otherwise. Unless defined otherwise, all technical and scientific terms used herein have the same meanings as commonly understood by one of ordinary skill in the art.

(10) The presently disclosed invention is a vessel useable in gravimetric methods for measuring the TDS or TS in a liquid sample. The vessel includes a main body formed of a thin wall polymeric film or material. Some non-limiting examples of polymeric materials include polyolefin films, such as polyethylene including high density polyethylene (HDPE), linear low density polyethylene (LLDPE), or low density polyethylene (LDPE); ethylene copolymers, such as ethylene vinyl acetate (EVA) copolymers or ethylene methyl acrylate (EMA) copolymer, polyethylene terephthalate (PET), polyethylene terephthalate glycol (PETG) copolymer; polypropylenes (PP), polyethylene-propylene copolymers; polymers and copolymers of polyvinyl chloride (PVC), polyvinylidene chloride (PVDC); nylon; thermoplastic elastomers such as styrenic block copolymers, polyolefin blends, elastomeric alloys, thermoplastic polyurethanes, thermoplastic copolyesters and thermoplastic polyamides; cellulose acetates; ionomer (Surlyn); polystyrene; polycarbonates; styrene acrylonitrile; aromatic polyesters; linear polyesters; thermoplastic polyvinyl alcohols; metalized films, such as metalized BoPET; and combinations thereof.

(11) In preferred embodiments, the polymeric material may be any material capable of being formed into a thin film which may withstand temperatures of at least 180 C. without melting or deforming. The film may have a thickness of less than 0.01 inches, preferably less than 0.008 inches, and more preferably less than 0.006 inches.

(12) In certain embodiments, the vessel may be a bag or cup formed by conventional cast or blown film processes. Alternatively, the vessel may be thermally formed from a high temperature polymeric film. The vessel may be formed to be flexible or may be formed to have non-flexible or low flexibility walls, or portions thereof, which may allow the vessel to be self-supporting. Further, in various embodiments, the vessel may be formed of flexible materials and may have a flat bottom which may allow the vessel to be self-standing.

(13) In preferred embodiments, the vessel may be a bag that is thermally formed from thin walled polymeric films having a melting temperature greater than 180 C. Some non-limiting examples of such preferred high temperature polymeric films include at least nylon, polyethylene terephthalate, polyethylene, and polypropylene. In embodiments, the vessel may have a total weight of less than 5.0 grams, such as between 0.5 grams and 5.0 grams.

(14) Referring now to the drawings, various embodiments of the thin film high temperature polymeric vessel of the presently disclosed invention are shown in FIGS. 1 through 3. FIG. 1 illustrates an embodiment of the vessel 10 having a flat bottom wall 16, longitudinally spaced opposing front and back walls 11, and connecting side walls 18 which allow the vessel to be self-standing. The vessel 10 further comprises an open top end 12 through which a liquid sample 14 may be deposited. As shown in FIG. 1, the bottom wall 16 and/or side walls 18 may be foldable so that the vessel 10 may be stored in a flat configuration. As such, many vessels may be packed together for shipping and sale, and may be easily stored in a small laboratory storage space.

(15) FIG. 2 illustrates an embodiment of the vessel 20 having gusseted side walls 28 and a bottom wall 26 which allows the vessel to be self-standing. The vessel further comprises an open top 22 through which a liquid sample 24 may be deposited. As described above, the bottom wall 26 may be folded so that the vessel 20 may be stored in a flat configuration.

(16) FIG. 3 illustrates another embodiment of the vessel 30 having a sealed bottom edge 36 and an open top edge 32 through which a liquid sample 34 may be deposited. The vessel 30 may be formed to have any number of wall portions, such as a front wall portion 31, a back wall portion 33, and side wall portions 38 as shown in FIG. 3. In certain embodiments, the vessel may be formed from a tube of high temperature thin walled polymeric material which is open along a top edge and folded and sealed along a bottom edge, or simply sealed along a bottom edge. As shown in FIG. 3, the vessel may not be self-standing but may need to be supported during use within a frame or other upstanding support such as, for example, a beaker.

(17) As discussed above, the vessels and bags of the presently disclosed invention may be produced from any polymeric material capable of being formed into a thin film, and thus provide for a vessel having an overall weight that is significantly lower than that of the prior art ceramic containers used in TDS testing. The lower weight (and corresponding lower overall volume) allows for less potential absorption of atmospheric moisture and thus better weight stability. Weight stability is important during TDS and TS testing to attain high accuracy results.

(18) The traditional containers used in testing TDS and/or TS typically weigh in excess of 50 grams, while the desired testing range for TDS is limited to a maximum of 200 mg. This large difference between the tested solid material weight and the weight of the container can cause resolution errors in determining the final weight of the solid material. In various embodiments of the presently disclosed invention, the total weight of the vessel may be between about 0.5 grams and about 5.0 grams. The lower weight of the vessel reduces the amount of moisture that may be absorbed, as discussed above, and consequently reduces the number of preconditioning steps required to achieve a stable tare weight.

(19) Embodiments of the vessels and bags of the presently disclosed invention may have a tare weight marked thereon. That is, the vessel or bag may have an indicia applied to a portion of the main body, wherein the indicia include a tare weight of the vessel which is the weight of the vessel recorded after at least one preconditioning step. In certain embodiments, the tare weight of the vessel may be the weight of the vessel recorded after at least two preconditioning steps.

(20) Each preconditioning step includes heating the vessel or bag to a high temperature for a specified time. The temperature may be about 180 C. and the time may be about an hour. The preconditioning step may include heating the vessel to at least 180 C. for a time greater than one hour, such as at least 6 hours, preferably at least 12 hours.

(21) In certain embodiments, the preconditioning step may further include weighing the vessel after the step of heating the vessel. As mentioned above, the tare weight of the vessel may be the weight of the vessel recorded after at least one preconditioning step.

(22) In certain embodiments, the weight of the vessel recorded after each preconditioning step may be compared to a weight recorder from a previous preconditioning step. If these weights vary by less than 0.5 mg, the last recorded weight may be the tare weight of the vessel. That is, the tare weight may not be recorded until subsequent preconditioning steps yields a variance of less than 0.5 mg. In certain embodiments, the tare weight may be recorded after subsequent preconditioning steps yields a variance of less than 0.1 mg, or even 0.05 mg. As such, the vessels and bags of the presently disclosed invention provide an accuracy and convenience that far exceeds that of the prior art vessels.

(23) The vessel of the presently disclosed invention may also be used to test the moisture content of a solid sample. As indicated above for the liquid sample, the vessels may have a tare weight indicated thereon. A solid sample may be placed in the vessel and the weight of the vessel containing the solid sample may be recorded. The vessel may be heated to evaporate liquid from the solid sample, and the vessel may then be reweighed. The change in weights may be used to determine the moisture content of the solid sample. In certain embodiments of this method, the vessel may be preconditioned prior to use to ensure a stable tare weight for the vessel.

(24) An alternate embodiment of the vessels and bags of the presently disclosed invention includes forming a moisture barrier coating on an inner surface, outer surface, or both inner and outer surfaces of the vessel to further aid in the weight stability by reducing moisture absorption. Alternatively, a metalized polymeric material such as, for example, metalized BoPET film may be used as the raw material for the vessel. Metalized polymeric films are very light weight and exhibit little to no moisture absorption over time. Thus, fewer or no preconditioning steps may be needed to record an accurate and stable tare weight for the vessel.

EXAMPLES

(25) Vessels formed according to embodiments of the presently disclosed invention were used for TDS testing according the protocols described in ASTM D5907 or Standard Methods 2540 B, C, or D as listed in the Code of Federal Regulations (40 CFR 136.3) or USGS I-1750-85. These protocols are periodically updated with changes to the methods and/or protocol numbers. Thus, while specific protocol numbers and method details have been listed herein, the vessels and methods of the presently disclosed invention may find utility in methods beyond those listed. For example, the vessels may be used in methods which require heating temperatures greater than 180 C., such as greater than 200 C., or even greater than 225 C. Furthermore, typical volumes contained within the vessel are listed herein as less than 500 mL, preferably less than 150 mL. Changes in standard methods may require that greater or lesser volumes of sample are tested. As such, the vessels of the presently disclosed invention may be configured to accommodate various ranges of sample volume, such as greater than 500 mL or less than 150 mL. While the film thickness may remain the same, the total weight of the vessel may be increased or reduced in parallel with the overall change in size of the vessel.

(26) Vessels according to embodiments of the presently disclosed invention were tested using the following protocol: (1) Vessels were preconditioned by (a) heating for one hour at 180 C., and (b) weighing the vessel. Steps 1(a) and 1(b) were repeated until a subsequently measured weight differed by less than 0.5 mgs from a previously measured weight. Typically, this occurred within two rounds of heating/weighing, wherein the final measured weight was recorded as the tare weight of the vessel. (2) A liquid sample containing a defined amount of solids was then added to a preconditioned vessel: for the examples shown below, 25-100 mL of water containing a known amount of KCl. (3) The vessel was then heated at 104 C. for a length of time sufficient to evaporate all of the liquid: for the examples shown below, the samples were heated overnight. (4) The vessel was then heated at 180 C. for 1 hour and weighed using a scale capable of 0.1 mg resolution. (5) Step 4 was repeated until two consecutively measured weights were within 0.0005 grams (0.5 mg). This last measured weight was the final recorded weight. (6) The final recovered solids weight was calculated as the final recorded weight of the vessel minus the tare weight of the vessel.

Example A

(27) Both nylon and PET materials were used to form a thin film vessel according to the configuration shown in FIG. 3. A specific weight of KCl was dissolved in water and placed in each of the testing vessels (column labeled Total Dissolved Solids Standard Weight (mg)). The liquid was evaporated and the weight of the vessel was recorded after two preconditioning steps. The results from this TDS Standard testing are listed in Table 1. Both PET and Nylon vessels showed excellent recoveries. In addition, a low weight trial of 5 mg (trial #5) was performed and showed similar recovery percentages.

(28) TABLE-US-00001 TABLE 1 Total Dissolved Solids standard testing recoveries using thin wall polymeric vessels Initial Total Dissolved Vessel Total Dissolved Solids Trial Vessel Weight Solids Standard Recovered No. Material (grams) Weight (mg) Weight (mg) % Recovery 1 PET 0.53724 167 167.1 100.06% 2 Nylon 0.6867 160.4 160.3 99.94% 3 Nylon 0.46314 148 149.26 100.85% 4 Nylon 4.54338 142.2 141.43 99.46% 5 Nylon 2.2803 5.04 5.1 101.19%

Example B

(29) Nylon vessels having a tare weight of less than 1 gram were tested for a range of standard weight recoveries which include standard weight samples comprising low (less than 100 mg), medium (between 100 mg and 150 mg), and high (greater than 150 mg) solids content. A control (blank) was included for several of the testing series, wherein the blank comprised water only. A standard test was considered successful (passed) if the final weight was within 10% (100%10%), while a control (blank) test was considered successful if the final weight was within 0.01 grams of the tare weight.

(30) Results from TDS testing Test using low weight samples of 10 mg are shown in Table 2, and low weight samples of about 25 mg are shown in Tables 3 and 4. Additional testing was performed by a testing laboratory according to the same protocol using nylon vessels as described herein. Results from high weight trials (200 mg) are shown in Tables 5 and 6, results from medium weight trials (100 mg) are shown in Tables 7 and 8, and results from low weight trials (10 mg) are shown in Table 9. In all, the majority of vessels tested showed a TDS recovery percent within the pass parameterswithin 10% of the standard weight measured.

(31) While specific embodiments of the invention have been described in detail, it should be appreciated by those skilled in the art that various modifications and alternations and applications could be developed in light of the overall teachings of the disclosure. Accordingly, the particular arrangements, systems, apparatuses, and methods disclosed are meant to be illustrative only and not limiting as to the scope of the invention.

(32) TABLE-US-00002 TABLE 2 Total Dissolved Solids standard test - low weight trials (~10 mg) Oven Temp ( C.) 104 180 180 Oven Time (min) 960 60 60 Tare Weight Weight Weight Bag Weight 1 2 3 Recovered Percent Number (g) (g) (g) (g) Weight (g) Recovered 1 0.64240 0.65508 0.65345 0.65315 0.01075 100.37% 2 0.64297 0.65581 0.65410 0.65370 0.01073 100.19% 3 0.64440 0.65690 0.65454 0.65444 0.01004 93.74% 4 0.64909 0.66210 0.65920 0.65943 0.01034 96.55% 5 0.63524 0.64810 0.64651 0.64641 0.01117 104.30% 6 0.64150 0.65360 0.65272 0.65242 0.01092 101.96% 7 0.64395 0.65625 0.65459 0.65414 0.01019 95.14% 8 0.64517 0.65799 0.65745 0.65749 0.01232 115.03% 9 0.64803 0.66170 0.66008 0.65959 0.01156 107.94% 10 0.64491 0.65836 0.65673 0.65626 0.01135 105.98% 11 0.64883 0.66210 0.66012 0.65963 0.01080 100.84% 12 0.63949 0.65310 0.65079 0.65054 0.01105 103.17% 13 0.64755 0.65841 0.65782 0.65760 0.01005 93.84% 14 0.64554 0.66325 0.65604 0.65596 0.01042 97.29% 15 0.65034 0.66380 0.66235 0.66189 0.01155 107.84% 17 0.65980 0.67360 0.67197 0.67159 0.01179 110.08% 18 0.64909 0.66080 0.65883 0.65900 0.00991 92.53% 19 0.64087 0.65404 0.65233 0.65192 0.01105 103.17% 22 0.65541 0.66901 0.66649 0.66616 0.01075 100.37% 23 0.66013 0.67350 0.67054 0.67029 0.01016 94.86% Standard: 25 ml water containing 0.01071 grams KCl

(33) TABLE-US-00003 TABLE 3 Total Dissolved Solids standard test - low weight trials (~25 mg) Oven Temp ( C.) 104 180 180 Oven Time (min) 960 60 60 Tare Weigh Weigh Weigh Bag Weight 1 2 3 Recovered Percent Number (g) (g) (g) (g) Weight (g) Recovered 25 0.65795 0.68405 0.68409 0.68360 0.02565 100.04% 26 0.65288 0.67915 0.67920 0.67896 0.02608 101.72% 27 0.65787 0.68389 0.68370 0.68356 0.02569 100.20% 28 0.65539 0.68200 0.68188 0.68149 0.02610 101.79% 29 0.66316 0.68925 0.68837 0.68830 0.02514 98.05% 30 0.65775 0.68350 0.68349 0.68309 0.02534 98.83% 31 0.65629 0.68149 0.68270 0.68189 0.02560 99.84% 32 0.65690 0.68245 0.68219 0.68173 0.02483 96.84% 33 0.65653 0.68230 0.68215 0.68177 0.02524 98.44% 34 0.65009 0.67595 0.67528 0.67534 0.02525 98.48% 35 0.64789 0.67390 0.67350 0.67374 0.02585 100.82% 36 0.65338 0.67849 0.67835 0.67819 0.02481 96.76% 37 0.65025 0.67575 0.67582 0.67561 0.02536 98.91% 38 0.65191 0.67710 0.67750 0.67738 0.02547 99.34% 39 0.65706 0.68235 0.68246 0.68225 0.02519 98.24% 40 0.65399 0.67945 0.67989 0.67975 0.02576 100.47% 41 0.66295 0.68875 0.68856 0.68815 0.02520 98.28% 42 0.66134 0.68760 0.68765 0.68729 0.02595 101.21% 43 0.66074 0.68673 0.68698 0.68649 0.02575 100.43% 44 0.66009 0.68635 0.68679 0.68635 0.02626 102.42% 45 0.66013 0.68429 0.68421 0.68401 0.02388 93.14% 46 0.65735 0.68270 0.68218 0.68236 0.02501 97.54% 47 0.64852 0.67465 0.67435 0.67397 0.02545 99.26% 48 0.66251 0.68795 0.68817 0.68785 0.02534 98.33% Standard: 25 ml water containing 0.02565 grams KCl

(34) TABLE-US-00004 TABLE 4 Total Dissolved Solids standard testing recoveries - Low Weight Trials (~25 mgs) Oven temp ( C.) 104 180 180 180 180 Oven time (min) 960 60 60 60 60 Tare Weigh 1 Weigh 2 Weight 3 Weigh 4 Weigh 5 Recovered Percent Bag Number Weight (g) (g) (g) (g) (g) (g) Weight (g) Recovered 51 0.63621 0.66133 0.66075 0.66130 0.66092 NA 0.02471 98.37% 52 0.62161 0.64698 0.64667 0.64696 NA NA 0.02535 100.92% 53 0.62361 0.64897 0.64879 0.64884 NA NA 0.02523 100.44% 54 0.62438 0.65008 0.65002 0.65011 NA NA 0.02573 102.43% 55 0.62448 0.64998 0.64978 0.64987 NA NA 0.02539 101.08% 56 0.62236 0.64740 0.64721 0.64770 NA NA 0.02534 100.88% 57 0.63036 0.65772 0.65745 0.65767 NA NA 0.02731 108.72% 58 0.62508 0.65078 0.65100 0.65111 NA NA 0.02603 103.63% 59 0.61005 0.63525 0.63547 0.63585 NA NA 0.02580 102.71% 60 0.61190 0.63754 0.63772 0.63795 NA NA 0.02605 103.71% 61 0.63941 0.66532 0.66485 0.66538 0.66488 NA 0.02547 101.40% 62 0.61512 0.64127 0.64112 0.64150 NA NA 0.02638 105.02% 63 0.62531 0.65158 0.65097 0.65161 0.65121 NA 0.02590 103.11% 64 0.62797 0.65428 0.65378 0.65495 0.65365 0.65379 0.02582 102.79% 65 0.62538 0.65180 0.65143 0.65179 NA NA 0.02641 105.14% 66 0.62752 0.65438 0.65433 0.65456 NA NA 0.02704 107.65% 67 0.63192 0.65879 0.65806 0.65882 0.65824 0.65855 0.02663 106.02% 68 0.62849 0.65529 0.65499 0.65527 NA NA 0.02678 106.61% 69 0.63686 0.66347 0.66305 0.66350 NA NA 0.02664 106.06% 70 0.63526 0.66196 0.66208 0.66235 NA NA 0.02709 107.85% 71 0.63264 0.65887 0.65895 0.65918 NA NA 0.02654 105.66% 72 0.64986 0.67615 0.67541 0.67636 0.67594 NA 0.02608 103.83% Standard: 25 ml water containing 0.02565 grams KCl NAnot applicable; measured difference in weight between last two readings less than 0.5 mg.

(35) TABLE-US-00005 TABLE 5 Total Dissolved Solids standard testing recoveries - High Weight Trials Sample Volume Initial wt Final Final Final Final Final wt (g) Final TDS Percent (mg) (mL) Bag # (g) wt (g) 1 wt (g) 2 wt (g) 3 wt (g) 4 wt (g) 5 used difference (g) recovery blank 100 39 0.64499 0.6449 0.6466 0.6417 0.6415 NA 0.6415 0.0002 0.0035 0.35% 200.515 50 106 0.62887 0.8392 0.83 0.8269 0.8273 NA 0.8273 0.0004 0.1984 98.96% 200.515 50 107 0.6278 0.828 0.8296 0.8291 NA NA 0.8291 0.0005 0.2013 100.39% 200.515 50 108 0.63299 0.8323 0.8336 0.831 0.8325 0.8322 0.8322 0.0003 0.1992 99.35% 200.515 50 109 0.6316 0.832 0.8341 0.83 0.8295 NA 0.8295 0.0005 0.1979 98.70% 200.515 50 110 0.63649 0.8361 0.8383 0.834 0.8338 NA 0.8338 0.0002 0.1973 98.40% 200.515 50 111 0.64226 0.8413 0.844 0.8402 0.8397 NA 0.8397 0.0005 0.1974 98.47% 200.515 50 112 0.63869 0.837 0.8387 0.8359 0.8355 NA 0.8355 0.0004 0.1968 98.15% 200.515 50 113 0.64136 0.8394 0.8405 0.8369 0.838 0.8381 0.8381 0.0001 0.1967 98.12% 200.515 50 114 0.64696 0.8472 0.8472 NA NA NA 0.8472 0 0.2002 99.86% 200.515 50 115 0.64241 0.841 0.8411 NA NA NA 0.8411 0.0001 0.1987 99.09% 200.515 50 116 0.63333 0.8316 0.832 NA NA NA 0.832 0.0004 0.1987 99.08% 200.515 50 118 0.6386 0.8356 0.8382 0.833 0.8325 NA 0.8325 0.0005 0.1939 96.70% Standard: 4.0103 mg/mL NAnot applicable; measured difference in weight between last two readings less than 0.5 mg.

(36) TABLE-US-00006 TABLE 6 Total Dissolved Solids standard testing recoveries - High Weight Trials Sample Volume Initial wt Final Final Final Final Final wt (g) Final Percent (mg) (mL) Bag # (g) wt (g) 1 wt (g) 2 wt (g) 3 wt (g) 4 wt (g) 5 used difference TDS (g) recovery blank 50 48 0.64503 0.644 0.6453 0.6422 0.642 NA 0.642 0.0002 0.003 0.30% 200.99 50 47 0.64934 0.8517 0.8517 NA NA NA 0.8517 0 0.2024 100.68% 200.99 50 49 0.64335 0.8501 0.8511 0.8477 0.8472 NA 0.8472 0.0005 0.2039 101.42% 200.99 50 50 0.63985 0.8459 0.8455 NA NA NA 0.8455 0.0004 0.2057 102.32% 200.99 50 51 0.6324 0.8382 0.836 0.8372 0.8367 NA 0.8367 0.0005 0.2043 101.65% 200.99 50 52 0.63511 0.8403 0.8371 0.838 0.8377 NA 0.8377 0.0003 0.2026 100.80% 200.99 50 53 0.6284 0.8333 0.8325 0.8327 NA NA 0.8327 0.0002 0.2043 101.65% 200.99 50 54 0.63605 0.8417 0.8412 NA NA NA 0.8412 0.0005 0.2052 102.07% 200.99 50 55 0.6428 0.8481 0.846 0.8461 NA NA 0.8461 0.0001 0.2033 101.15% 200.99 50 56 0.63975 0.8431 0.8426 NA NA NA 0.8426 0.0005 0.2029 100.93% 200.99 50 57 0.64083 0.8444 0.8453 0.8453 NA NA 0.8453 0 0.2045 101.73% 200.99 50 59 0.63549 0.8375 0.8403 0.8376 0.8371 NA 0.8371 0.0005 0.2016 100.31% 200.99 50 60 0.63218 0.8355 0.835 NA NA NA 0.835 0.0005 0.2028 100.91% 200.99 50 61 0.63466 0.8373 0.8385 0.8372 0.8367 NA 0.8367 0.0005 0.202 100.52% 200.99 50 62 0.64063 0.8422 0.8425 NA NA NA 0.8425 0.0003 0.2019 100.44% 200.99 50 63 0.63525 0.8371 0.8372 NA NA NA 0.8372 0.0001 0.202 100.48% 200.99 50 64 0.63613 0.8411 0.8426 0.8402 0.8405 NA 0.8405 0.0003 0.2044 101.68% 200.99 50 65 0.63391 0.8352 0.8348 NA NA NA 0.8348 0.0004 0.2009 99.95% 200.99 50 66 0.62868 0.8335 0.8343 0.834 NA NA 0.834 0.0003 0.2053 102.15% 200.99 50 67 0.63269 0.8369 0.8386 0.8323 0.8348 0.8343 0.8343 0.0005 0.2016 100.31% 200.99 50 68 0.6323 0.8375 0.8384 0.8318 0.8319 NA 0.8319 0.0001 0.1996 99.31% 200.99 50 69 0.6538 0.8572 0.8585 0.8519 0.8515 NA 0.8515 0.0004 0.1977 98.36% 200.99 50 70 0.6376 0.8412 0.842 0.8416 NA NA 0.8416 0.0004 0.204 101.50% Standard: 4.0198 mg/mL

(37) TABLE-US-00007 TABLE 7 Total Dissolved Solids standard testing recoveries - Medium Weight Trials Sample Volume Initial Final Final Final Final wt (g) Final Percent (mg) (mL) Bag # wt (g) wt (g) 1 wt (g) 2 wt (g) 3 wt (g) 4 used difference TDS (g) recovery blank 50 121 0.64732 0.6476 0.6461 0.6466 NA 0.6466 0 0.0007 0.07% 100.205 50 122 0.64692 0.7492 0.7477 0.7473 NA 0.7473 0.0004 0.1004 100.17% 100.205 50 123 0.64621 0.7462 0.7457 NA NA 0.7457 0.0005 0.0995 99.29% 100.205 50 124 0.63899 0.7388 0.7384 NA NA 0.7384 0.0004 0.0994 99.21% 100.205 50 125 0.63319 0.7319 0.7323 NA NA 0.7323 0.0004 0.0991 98.91% 100.205 50 126 0.64529 0.7509 0.7438 0.7434 NA 0.7434 0.0004 0.0981 97.91% 100.205 50 127 0.65533 0.7575 0.7544 0.754 NA 0.754 0.0004 0.0987 98.47% 100.205 50 128 0.65111 0.7533 0.7479 0.7474 NA 0.7474 0.0005 0.0963 96.09% 100.205 50 129 0.64583 0.7459 0.7428 0.7425 NA 0.7425 0.0003 0.0967 96.47% 100.205 50 130 0.64998 0.7483 0.7465 0.746 NA 0.746 0.0005 0.096 95.82% 100.205 50 131 0.65568 0.7534 0.7532 NA NA 0.7532 0.0002 0.0975 97.32% 100.205 50 132 0.64883 0.7497 0.7458 0.7468 0.7466 0.7466 0.0002 0.0978 97.57% 100.205 50 133 0.65163 0.754 0.7506 0.7475 0.748 0.748 0.0005 0.0964 96.17% 100.205 50 134 0.65401 0.7592 0.7505 0.7502 NA 0.7502 0.0003 0.0962 95.99% 100.205 50 135 0.64929 0.7554 0.746 0.7456 NA 0.7456 0.0004 0.0963 96.11% 100.205 50 136 0.6503 0.7492 0.7471 0.7469 NA 0.7469 0.0002 0.0966 96.40% 100.205 50 137 0.65167 0.7496 0.7486 0.7487 NA 0.7487 0.0001 0.097 96.83% 100.205 50 138 0.63879 0.7365 0.7354 0.7349 NA 0.7349 0.0005 0.0961 95.91% 100.205 50 139 0.63492 0.7317 0.7321 NA NA 0.7321 0.0004 0.0972 96.98% 100.205 50 140 0.65061 0.7503 0.7466 0.7463 NA 0.7463 0.0003 0.0957 95.49% 100.205 50 141 0.6572 0.7573 0.7522 0.7522 NA 0.7522 0 0.095 94.81% 100.205 50 142 0.64917 0.7478 0.746 0.7455 NA 0.7455 0.0005 0.0963 96.13% 100.205 50 143 0.64966 0.7464 0.7459 NA NA 0.7459 0.0005 0.0962 96.04% 100.205 50 144 0.65333 0.7504 0.7499 NA NA 0.7499 0.0005 0.0966 96.37% Standard: 2.0041 mg/mL

(38) TABLE-US-00008 TABLE 8 Total Dissolved Solids standard testing recoveries - Medium Weight Trials Sample Volume Initial Final Final Final Final wt (g) Final Percent (mg) (mL) Bag # wt (g) wt (g) 1 wt (g) 2 wt (g) 3 wt (g) 4 used difference TDS (g) recovery blank 50 170 0.63772 0.6353 0.6353 NA NA 0.6353 0 0.0024 0.24% 100.415 50 171 0.63185 0.7276 0.7277 NA NA 0.7277 0.0001 0.0959 95.45% 100.415 50 172 0.63739 0.7369 0.7393 0.7382 0.7382 0.7382 0 0.1008 100.39% 100.415 50 173 0.6246 0.7225 0.72 0.7197 NA 0.7197 0.0003 0.0951 94.71% 100.415 50 174 0.62652 0.723 0.7233 NA NA 0.7233 0.0003 0.0968 96.38% 100.415 50 175 0.63025 0.7268 0.7265 NA NA 0.7265 0.0003 0.0963 95.85% 100.415 50 176 0.64325 0.7373 0.7377 NA NA 0.7377 0.0004 0.0945 94.06% 100.415 50 177 0.64741 0.737 0.7366 NA NA 0.7366 0.0004 0.0892 88.82% 100.415 50 178 0.64143 0.7432 0.7434 NA NA 0.7434 0.0002 0.102 101.55% 100.415 50 179 0.63314 0.7295 0.7292 NA NA 0.7292 0.0003 0.0961 95.66% 100.415 50 180 0.6147 0.7217 0.7225 0.7222 NA 0.7222 0.0003 0.1075 107.06% 100.415 50 181 0.6376 0.7326 0.7328 NA NA 0.7328 0.0002 0.0952 94.81% 100.415 50 182 0.63718 0.7307 0.7308 NA NA 0.7308 0.0001 0.0936 93.23% 100.415 50 183 0.63697 0.7298 0.7295 NA NA 0.7295 0.0003 0.0925 92.15% 100.415 50 184 0.64373 0.736 0.736 NA NA 0.736 0 0.0923 91.89% 100.415 50 185 0.64055 0.7342 0.7344 NA NA 0.7344 0.0002 0.0939 93.46% 100.415 50 186 0.64771 0.7403 0.7408 NA NA 0.7408 0.0005 0.0931 92.71% 100.415 50 187 0.63534 0.7268 0.7265 NA NA 0.7265 0.0003 0.0912 90.78% 100.415 50 188 0.6308 0.7232 0.7233 NA NA 0.7233 0.0001 0.0925 92.12% 100.415 50 189 0.6319 0.7208 0.7203 NA NA 0.7203 0.0005 0.0884 88.03% 100.415 50 190 0.63155 0.7236 0.724 NA NA 0.724 0.0004 0.0925 92.07% 100.415 50 191 0.63344 0.7232 0.7234 NA NA 0.7234 0.0002 0.09 89.59% 100.415 50 192 0.63604 0.7294 0.7294 NA NA 0.7294 0 0.0934 92.97% Standard: 2.0083 mg/mL

(39) TABLE-US-00009 TABLE 9 Total Dissolved Solids standard testing recoveries - Low Weight Trials Sample Volume Initial Final Final Final wt (g) Final TDS Percent (mg) (mL) Bag # wt (g) wt (g) 1 wt (g) 2 wt (g) 3 used difference (g) Recovery 10.03 50 301 0.60837 0.6193 0.6191 NA 0.6191 0.0002 0.0107 106.98% 10.03 50 305 0.6066 0.6163 0.6159 NA 0.6159 0.0004 0.0093 92.72% 10.03 50 306 0.60002 0.6067 0.6104 0.6101 0.6101 0.0003 0.0101 100.50% 10.03 50 307 0.60193 0.6117 0.6117 NA 0.6117 0 0.0098 97.41% 10.03 50 308 0.61248 0.622 0.6222 NA 0.6222 0.0002 0.0097 96.91% 10.03 50 309 0.61932 0.6293 0.6282 0.6282 0.6282 0.0089 0.0089 88.53% 10.03 50 310 0.60518 0.6137 0.6141 NA 0.6141 0.0004 0.0089 88.93% 10.03 50 311 0.61292 0.6258 0.6236 0.6233 0.6233 0.0003 0.0104 103.49% Standard: 0.2006 mg/mL