JPH0359451A - Method for measuring concentration of primary ammonium phosphate - Google Patents
Method for measuring concentration of primary ammonium phosphateInfo
- Publication number
- JPH0359451A JPH0359451A JP19394289A JP19394289A JPH0359451A JP H0359451 A JPH0359451 A JP H0359451A JP 19394289 A JP19394289 A JP 19394289A JP 19394289 A JP19394289 A JP 19394289A JP H0359451 A JPH0359451 A JP H0359451A
- Authority
- JP
- Japan
- Prior art keywords
- end point
- stage
- point
- change
- determined
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 16
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 7
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 7
- 239000006012 monoammonium phosphate Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 8
- 235000011149 sulphuric acid Nutrition 0.000 abstract description 6
- 238000004448 titration Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000012790 confirmation Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- VKFFEYLSKIYTSJ-UHFFFAOYSA-N tetraazanium;phosphonato phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])([O-])=O VKFFEYLSKIYTSJ-UHFFFAOYSA-N 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 239000005696 Diammonium phosphate Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野１
本発明は、コークス炉ガスよりアンモニアを除去するた
めの）オサム法において用いる吸収液（第１リン酸アン
モニウム（ＮＨ４１ＨｚＰＯ＋）の濃度の測定方法に関
するものである。Detailed Description of the Invention [Industrial Application Field 1] The present invention relates to a method for measuring the concentration of an absorption liquid (ammonium monophosphate (NH41HzPO+)) used in the Osamu method (for removing ammonia from coke oven gas). It is something.
［従来の技術］
コークス炉ガス（ＣＯＣｌ よりアンモニアを除去する
ための）オサム法で用いる吸収液である第１リン酸アン
モニウム（ＮＨ，１Ｈ２Ｐ０４の濃度測定方法として従
来次の方法が知られている。[Prior Art] The following method is conventionally known as a method for measuring the concentration of diammonium phosphate (NH, 1H2P04), which is an absorption liquid used in the Osamu method for removing ammonia from coke oven gas (COCl).
それは、硫酸（Ｈ２ＳＯ４）並びに水酸化ナトリウムｌ
Ｎａ口旧の標準液により電位差滴定により行なわれる、
即ち、まず酸量の（例えば２ａ＋１の）試料を採取し、
一定量（例えば５０ｏ＋１）の稀釈水でサンプル計量器
の洗浄も兼ねて稀釈し滴定セルへ送る。It contains sulfuric acid (H2SO4) as well as sodium hydroxide l
Performed by potentiometric titration with Na standard solution.
That is, first take a sample with an acid amount (for example, 2a+1),
The sample is diluted with a certain amount (for example, 50°+1) of dilution water, which also serves as a wash for the sample measuring device, and sent to the titration cell.
この試料をＨ２ＳＯ４、ＮａＯＨ標準液で滴定する。This sample is titrated with H2SO4, NaOH standard solution.
最初にＨａＳＯ，で滴定すると、Ｈ２ＳＯ４は試料中の
第ニリン酸アンモニウムと（１）に示すように反応して
当量点においてＰＨが急変する。When first titrating with HaSO, H2SO4 reacts with ammonium diphosphate in the sample as shown in (1), causing a sudden change in pH at the equivalence point.
２ ｔｓｔ＋４＋ ＲＨＰＯａ＋Ｈ２ＳＯ４→２Ｎｌ（
ＪｔＰＯｌ” ｆＮＨ−） １ｓＯ４（ｔ１次に上の溶
液なＮａＯＨで滴定すると、Ｍａｉｌ（は溶液中の第一
リン酸アンモニウム（原試料中に存在していたものと反
応（１１によって生じたもの）と次の（２）に示すよう
に反応して当量点においてＰＨの急変が生ずる。2 tst+4+ RHPOa+H2SO4→2Nl(
JtPOl" fNH-) 1sO4 (t1) Then, when titrated with the above solution of NaOH, Mail( reacts with the monoammonium phosphate in the solution (that which was present in the original sample (formed by 11)). As shown in the following (2), the reaction causes a sudden change in pH at the equivalence point.
Ｎ１１４１１−ＰＯ＋Ｎａ０Ｈ＝ Ｎ）１４ＮａｌｌＰ
Ｏ＋＋ＨａＯ（２１上記のように反応させ夫々ＰＨの変
化ΔＰＨを求めその変化の大きい点（終点）を求め、こ
れにより吸収液である第ニリン酸アンモニウムの濃度を
測定する。N11411-PO+Na0H=N)14NallP
O++HaO (21) are reacted as described above, and the change in pH ΔPH is determined, the point where the change is large (end point) is determined, and the concentration of ammonium diphosphate, which is the absorption liquid, is measured.
［発明が解決しようとする課題］
第４図、第５図は、前記の滴定の際のＰＨの変化ΔＰＨ
の変化量を示すもので、第４図は１段目の終点付近、第
５図は２段目の終点付近のグラフである。つまりＲが１
段目の終点であり、Ｔが２段目の終点である。[Problems to be Solved by the Invention] Figures 4 and 5 show the change in pH ΔPH during the above titration.
4 is a graph near the end point of the first stage, and FIG. 5 is a graph near the end point of the second stage. That is, R is 1
This is the end point of the second stage, and T is the end point of the second stage.
ここで１段目においては、例えば第４図に示ずＲｏのよ
うに実際の終点Ｒよりも前の点を終点とすることがあり
、当量点との誤差が大きすぎて正確な測定が出来ない。Here, in the first stage, the end point may be a point before the actual end point R, such as Ro not shown in Figure 4, and the error with the equivalent point is too large to allow accurate measurement. do not have.
又２段目の場合変化が比較的ゆるやかであるためΔＰＨ
が１デジツト以下になりΔＰＨが変化しなくなりＮａＯ
Ｈが高いところを終点とし正確な測定が出来なくなる。In addition, in the case of the second stage, since the change is relatively gradual, ΔPH
becomes less than 1 digit and ∆PH stops changing and NaO
The end point is a point where H is high, and accurate measurement becomes impossible.
つまり第５図においてＴｏを終点とする。That is, in FIG. 5, To is the end point.
以上の滴定におけるＰＨの変化を示したグラフが第１図
である。この図においてＲが１段目の急変点（終点）で
ありＴが２段目の急変点（終点）である。FIG. 1 is a graph showing the change in pH during the above titration. In this figure, R is the sudden change point (end point) of the first stage, and T is the sudden change point (end point) of the second stage.
このような滴定の結果から、次の式（３）、（４１を用
いて試料中のアンモニア、リン酸の各濃度を求めること
が出来る。From the results of such titration, the concentrations of ammonia and phosphoric acid in the sample can be determined using the following equations (3) and (41).
Ｎ１１４ （ａ＋ｏｌｌ ＝ （Ｌ Ｘ Ａ ＋ ｆ
ａＸ Ｂ ）／ｖ １３１ＨａＰ０４（ｗ
ａｌｌ＝ （ｆｘＸ Ｂ ｌ／ｖ
（４）ただし、Ａは１段目の終点までのＨａＳＯ４
の量（ｍｏｌｌ 、 Ｂは１段目の終点から２段目の終
点までのＮａ０１１の量（ｎ＋１１． ｆｌは＋ｔ、Ｓ
Ｏ４のファクター、ｆ２はＮａＯＨのファクター、■は
試料の採取量である。N114 (a+oll = (L X A + f
aX B )/v 131HaP04(w
all= (fxX B l/v
(4) However, A is HaSO4 up to the end point of the first stage
amount (mol), B is the amount of Na011 from the end point of the first stage to the end point of the second stage (n+11. fl is +t, S
The O4 factor, f2 is the NaOH factor, and ■ is the amount of sample collected.
したがって本発明は、１段目の終点のおよび２段目の終
点の決定に当たって、いずれも正しい点を終点として定
めることが正確に行なわれ得る第１リン酸アンモニウム
の濃度測定方法を提供する６のである。Therefore, the present invention provides a method for measuring the concentration of monoammonium phosphate that can accurately determine the correct point as the end point in determining the end point of the first stage and the end point of the second stage. be.
［課題を解決するための手段］
本発明の第一リン酸アンモニウムの濃度測定方法は、所
定量の１１□３０４を滴下し被測定液のＰＩＩの変化量
ΔＰＨを順次求め、ＰＨの急変点であるΔＰＨの大小関
係が変化する点をもって１段目の終点とし、次いで所定
量のＮａＯＨを滴下して被測定液のＰＳＩの変化量ΔＰ
Ｈを順次求め、ＰＨの急変点であるΔＰＨの大小関係の
変化する点をもって２段目の終点とし。[Means for Solving the Problems] The method for measuring the concentration of monoammonium phosphate of the present invention involves dropping a predetermined amount of 11□304, sequentially determining the amount of change ΔPH in PII of the liquid to be measured, and detecting the change at the point of sudden change in pH. The point at which the magnitude relationship of a certain ΔPH changes is defined as the end point of the first stage, and then a predetermined amount of NaOH is dropped to determine the amount of change ΔP in PSI of the liquid to be measured.
H is determined sequentially, and the point at which the magnitude relationship of ΔPH changes, which is a sudden change in PH, is set as the end point of the second stage.
これら１段目の終点および２段目の終点での液量にもと
づいて第一リン酸アンモニウムの濃度を測定するもので
、１段目の終点決定にあたって所定のＰＨ値以上のとこ
ろでのΔＰＨの大小関係が変化した点を１段目の終点と
するちのである。これによって第２図に示すように所定
ＰＨのＰｓの点よりｔＰＨが大である領域での急変点Ｒ
を終点として定めることが出来る。これによって、従来
の方法のようにＲｏを終点とすることを避けることが出
来る。The concentration of monoammonium phosphate is measured based on the liquid volume at the end point of the first stage and the end point of the second stage, and the magnitude of ΔPH at a predetermined pH value or higher is used to determine the end point of the first stage. The point where the relationship changes is set as the end point of the first stage. As a result, as shown in FIG.
can be set as the end point. This makes it possible to avoid setting Ro as the end point as in the conventional method.
又２段目の終点の決定にあたっては、ΔＰＨの大小関係
の変化が、第３図に示すような場合、その変化開始点Ｔ
１と変化終了点Ｔ２を求め５それらの中間点Ｔを終点と
するものである。In addition, when determining the end point of the second stage, if the change in the magnitude relationship of ΔPH is as shown in Figure 3, the change starting point T
1 and the change end point T2 are found, and the intermediate point T between them is set as the end point.
したがって、従来の方法のように第５図に示すＴｏを終
点とすることはなく、適切な終点の決定が可能である。Therefore, unlike the conventional method, To shown in FIG. 5 is not set as the end point, and an appropriate end point can be determined.
［実施例］
＋１１初期ＰＨの検出
滴定開始時のＰＨを測定し、試料が所定範囲内のＰＨで
あることを確認する。[Example] +11 Detection of initial pH The pH at the start of titration is measured and it is confirmed that the pH of the sample is within a predetermined range.
（２）１段目の終点検出
０、 Ｏｌａ＋ｌのＨ，Ｓ０４を滴下し、その都度のｌ
）Ｈの変化量をΔＰＨを夫々Ａ、、Ａ、＋、Ａ、、・・
・、 Ａ１．ｌ−１，Ａ＆ｌｌ Ａｖ＋＋Ａ、、、Ａ、
、Ａ□１とする。(2) First stage end point detection 0, Ola+l H, S04 is dropped, and each time
)H change amount and ΔPH are respectively A,, A, +, A,...
・, A1. l-1,A&ll Av++A,,,A,
, A□1.
ここでＡＩ＜Ａ、＜Ａ、＜・・・Ａｌｌ −＋ ＜ Ａ
ｌｌ ＞ Ａ、や、・・・ＡＭ−１＜Ａｓ＞Ａ、１４＋
であったとするとＡ４とＡｓがΔＰＨが大小関係が変化
する点として求められる。Here, AI<A, <A, <...All −+ <A
ll > A, Ya...AM-1<As>A, 14+
If this is the case, A4 and As can be found as points at which the magnitude relationship of ΔPH changes.
ここでＡＭ、 ＡＭの点でのＰＨを夫々ｐ、、 ｐ、と
する時、九＜Ｐｉ、 ＰＮ＞Ｐ、であれば、ＰＨがＰｖ
であるＡ２の点は終点とせず捨てる。そしてＰＨがＰ３
よりの大の１’Ｎの点Ａｎを１段目の終点とする。Here, when the PH at the points AM and AM are p, , p, respectively, if 9<Pi, PN>P, then PH is Pv
Point A2, which is , is not considered as the end point and is discarded. And the PH is P3
Let the point An of 1'N with the larger value be the end point of the first stage.
これをグラフで示したのが第２図である６つまりこの図
においてグラフ中ピークがＡ、とＡｎの二つあるが、そ
のうちのＰ、よりも大きいＰＨのＡ、の点が１段目の終
点である。This is shown in a graph in Figure 2.6 In other words, in this figure, there are two peaks in the graph, A and An, and the point A, which has a larger PH than P, is in the first row. It is the end point.
これに対して従来の方法においては第４図に示すように
グラフの最初のピークＡＭ（Ｔ’ｌを終点としてしまう
、そしてこの時の液量をもとにリン酸アンモニウムの濃
度を求めることになり誤まった値となる。On the other hand, in the conventional method, the end point is the first peak AM (T'l) of the graph as shown in Figure 4, and the concentration of ammonium phosphate is determined based on the liquid volume at this time. This will result in an incorrect value.
（３）２段目の終点の検出
１段目と同様に０．０１ｍ１のＮａＯＨを滴下し、その
時のＰＨの変化量ΔＰＨをり、Ｂｇ、・・・＋ＢＮ−１
＋ＢＮ＋ＢＮとする。(3) Detection of the end point of the second stage Drop 0.01 ml of NaOH in the same way as the first stage, and calculate the amount of change in PH at that time ΔPH, Bg,...+BN-1
+BN+BN.
ここで Ｂｌ＜８．＜−＜８Ｎ−１＜ Ｂｓ＞ Ｂｎｌ
となった場合は、ΔＰＨがＢＮの時の液量を終点の液量
とする。Here Bl<8. <-<8N-1<Bs> Bnl
In this case, the liquid volume when ΔPH is BN is set as the liquid volume at the end point.
又Ｂ＋ ＜ Ｂｚ＜ ・＝ ＜ Ｂ＋ａ＝ Ｂｕ−ｔ
＝ −＝ ＢＮ−１＜ Ｂｎ＜ ＢＮ＋１となった場合
は、ΔＰＨがＢ、の時の液量ＭとΔＰＨがＢＮの時の液
量Ｎから（Ｍ＋Ｎｌ／２を終点の液量とする。Also, B+ <Bz< ・= < B+a= But-t
= -= BN-1 < Bn < BN+1, from the liquid volume M when ΔPH is B and the liquid volume N when ΔPH is BN, (M+Nl/2 is taken as the liquid volume at the end point.
このように本実施例においては、２段目の終点として第
３図のＴを検出しその時の液量に相当する（Ｍ＋Ｎｌ
／２を液量としている。In this example, T in FIG. 3 is detected as the end point of the second stage, and corresponds to the liquid volume at that time (M+Nl
/2 is the liquid volume.
これに対し従来の方法では、第５図のＴ゛を終点とする
ことになる。In contrast, in the conventional method, T'' in FIG. 5 is the end point.
以上のようにして求めた１段目の終点と２段目の終点の
液量にもとづいて、既に述べた濃度検出のための基礎と
なる＋３１１４１式により第１リン酸アンモニウムの濃
度が決定される。Based on the liquid volumes at the end point of the first stage and the end point of the second stage determined as described above, the concentration of monoammonium phosphate is determined by the +31141 formula, which is the basis for concentration detection described above. .
［発明の効果］
以上述べたように、本発明の方法によれば、１段目の終
点の決定に際して試料のＰＨが所定の値以上の範囲内に
おいて定めることにしたので、他の要因によるＰＨの急
変点を終点とすることむしに正しい終点を求めることが
出来る。又２段目の終点の決定に際しては、変化の開始
と変化の終了の中間点を終点を定めることによって正し
い終点を求めることが出来る。これによって従来方法よ
りも精度の高い濃度測定が可能になる。[Effects of the Invention] As described above, according to the method of the present invention, when determining the end point of the first stage, it is determined that the pH of the sample is within a range of a predetermined value or higher, so that the pH due to other factors is not affected. It is possible to find the correct end point by taking the abrupt turning point as the end point. When determining the end point of the second stage, the correct end point can be determined by determining the end point as the midpoint between the start of the change and the end of the change. This makes it possible to measure concentration with higher accuracy than conventional methods.
第１図は本発明の方法の基本原理による測定時のＰＨの
変化を示したグラフ、第２図は本発明の方法による１段
目の終点の決定手段を示した図、第３図は本発明の方法
による２段目の終点の決定手段を示した図、第４図、第
５図は夫々従来方法の１段目、２段目における終点決定
手段を示す図である。FIG. 1 is a graph showing the change in pH during measurement according to the basic principle of the method of the present invention, FIG. 2 is a graph showing the means for determining the end point of the first stage according to the method of the present invention, and FIG. FIGS. 4 and 5 are diagrams showing end point determining means in the second stage according to the method of the invention, and FIGS. 4 and 5 are diagrams showing end point determining means in the first stage and second stage, respectively, of the conventional method.
Claims (2)
ＰＨの変化量を順次求め変化量の直前のものとの大小関
係が変化する点を１段目の終点とし、次いで所定量のＮ
ａＯＨを滴下してＰＨの変化量を順次求め変化量の直前
のものとの大小関係が変化する点を２段目の終点とし、
１段目の終点における液量と２段目の終点における液量
とから第１リン酸アンモニウムの濃度を測定する方法に
おいて、１段目の終点の決定の際にＰＨが特定の値以上
の時に生じた前記大小関係の変化点をもって１段目の終
点とすることを特徴とした濃度測定方法。(1) Drop a predetermined amount of H_2SO_4 into the liquid to be measured, sequentially calculate the amount of change in PH, set the point where the magnitude relationship with the previous one changes as the end point of the first stage, then add a predetermined amount of N
The amount of change in PH is sequentially determined by dropping aOH, and the point where the magnitude relationship with the previous amount of change changes is set as the end point of the second stage,
In the method of measuring the concentration of monoammonium phosphate from the liquid volume at the end point of the first stage and the liquid volume at the end point of the second stage, when the pH is above a specific value when determining the end point of the first stage. A concentration measuring method characterized in that the point of change in the magnitude relationship that occurs is taken as the end point of the first stage.
ＰＨの変化量を順次求め変化量の直前のものとの大小関
係が変化する点を１段目の終点とし、次いで所定量のＮ
ａＯＨを滴下してＰＨの変化量を順次求め変化量の直前
のものとの大小関係が変化する点を２段目の終点とし、
１段目の終点における液量と２段目の終点における液量
とから第１リン酸アンモニウムの濃度を測定する方法に
おいて、２段目の終点の決定の際に前記大小関係の変化
の開始点の液量と終了点の液量との平均液量をもって２
段目の終点の液量とすることを特徴とする濃度測定方法
。(2) Drop a predetermined amount of H_2SO_4 into the liquid to be measured, sequentially calculate the amount of change in PH, set the point at which the magnitude relationship with the one immediately before the change changes as the end point of the first stage, then add a predetermined amount of N
The amount of change in PH is sequentially determined by dropping aOH, and the point where the magnitude relationship with the previous amount of change changes is set as the end point of the second stage,
In the method of measuring the concentration of monoammonium phosphate from the liquid volume at the end point of the first stage and the liquid volume at the end point of the second stage, when determining the end point of the second stage, the starting point of the change in the magnitude relationship is determined. The average liquid volume between the liquid volume at the end point and the liquid volume at the end point is 2.
A concentration measuring method characterized by measuring the liquid volume at the end point of each stage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19394289A JPH0359451A (en) | 1989-07-28 | 1989-07-28 | Method for measuring concentration of primary ammonium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19394289A JPH0359451A (en) | 1989-07-28 | 1989-07-28 | Method for measuring concentration of primary ammonium phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0359451A true JPH0359451A (en) | 1991-03-14 |
Family
ID=16316311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19394289A Pending JPH0359451A (en) | 1989-07-28 | 1989-07-28 | Method for measuring concentration of primary ammonium phosphate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0359451A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9655435B2 (en) | 2008-12-15 | 2017-05-23 | Glaxosmithkline Consumer Healthcare Gmbh & Co., Kg | Toothbrush bristle arrangement |
-
1989
- 1989-07-28 JP JP19394289A patent/JPH0359451A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9655435B2 (en) | 2008-12-15 | 2017-05-23 | Glaxosmithkline Consumer Healthcare Gmbh & Co., Kg | Toothbrush bristle arrangement |
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